Hydroxylamine salt solventing-out crystallization device

Abstract

The hydroxylamine salt solvating-out crystallization device comprises a body, a feeding mechanism, a stirring mechanism, a temperature control layer and a discharging mechanism, the feeding mechanism comprises a first sealing cover and a solvating-out agent liquid distribution mechanism, the first sealing cover is communicated with a solvating-out agent feeding pipe, the solvating-out agent liquid distribution mechanism is divided into a fixing part and a liquid distribution part, and the fixing part is communicated with the solvating-out agent feeding pipe. Liquid outlet holes are formed in the inclined side wall and the bottom surface of the liquid distribution part, a second through hole is formed in the bottom of the liquid distribution part, the side wall of the upper end of the body is communicated with a mother liquid feeding pipe, the stirring mechanism penetrates through the second through hole to stir in the solventing-out agent liquid distribution mechanism and the body, and a solventing-out agent enters the crystallization device through the solventing-out agent feeding pipe; after being stirred by the stirring mechanism, the hydroxylammonium salt solution is uniformly distributed into the body through the liquid distribution part, and the hydroxylammonium salt solution enters the body through the mother liquor feeding pipe to be mixed with the solventing-out agent, so that hydroxylammonium salt crystals are separated out from the mother liquor. The crystallization device can uniformly distribute the solventing-out liquid into the mother liquid, and uniform crystal substances are separated out.

Description

TECHNICAL FIELD

[0001] The utility model relates to crystallization device technical field more specifically, relate to a kind of hydroxylamine salt solution crystallization device. BACKGROUND

[0002] Hydroxylamine salt crystallization is the key link of affecting its product quality in hydroxylamine industrial production process, and currently hydroxylamine salt crystallization can adopt solution crystallization, and solution crystallization is based on phase equilibrium principle, when adding solution agent to solution, the property of mixed solvent changes, and the chemical potential of solute in new mixed solvent increases.According to the relationship between chemical formula and solubility, the solubility of solute decreases.When the concentration of solute exceeds its saturation solubility in new mixed solvent, solute will be precipitated from solution in the form of crystal.The existing crystallizer drops solution agent using upper single-tube dropping method, which can cause uneven dropping, high local solution agent concentration, resulting in impure product and low yield.

[0003] The above problems are urgent to be solved, so the utility model provides a kind of hydroxylamine salt solution crystallization device for solving the above problems. UTILITY MODEL CONTENT

[0004] The technical problem to be solved by the utility model is to provide a kind of hydroxylamine salt solution crystallization, to solve the technical problems of uneven dropping of solution agent and high local solution agent concentration in prior art.

[0005] The technical scheme adopted by the utility model to solve its technical problem is to provide a kind of hydroxylamine salt solution crystallization device, which comprises a body, a feeding mechanism arranged at the top end of the body, a stirring mechanism arranged in the body, a temperature control layer arranged at the side of the body, and a discharging mechanism arranged at the bottom end of the body.The feeding mechanism comprises a first sealing cover and a solution agent liquid distribution mechanism, and the first sealing cover is connected with the solution agent feeding pipe.The solution agent liquid distribution mechanism is divided into a fixed part at the top and a liquid distribution part at the bottom.The fixed part is fixed between the first sealing cover and the body to fix the solution agent liquid distribution mechanism.The liquid distribution part is provided with liquid outlet holes on the inclined side wall and the bottom surface, and the bottom of the liquid distribution part is provided with a second through hole.The upper end of the body is connected with a mother liquor feeding pipe, and the stirring mechanism passes through the second through hole to stir in the solution agent liquid distribution mechanism and the body.The solution agent enters the crystallization device from the solution agent feeding pipe, is stirred by the stirring mechanism, and is then uniformly distributed in the body by the liquid distribution part.The hydroxylamine salt solution enters the body from the mother liquor feeding pipe, mixes with the solution agent, and makes the hydroxylamine salt crystallize from the mother liquor.

[0006] Preferably, the first limiting hole is uniformly arranged around the top end of the body, the second limiting hole is uniformly arranged around the bottom end of the body, the third limiting hole is uniformly arranged around the bottom end of the first sealing cover, the first through hole is arranged on the first sealing cover, the fourth limiting hole is arranged on the fixed part, and the bolt passes through the third limiting hole, the fourth limiting hole and the first limiting hole to fix the dissolving agent liquid distribution mechanism between the first sealing cover and the body.

[0007] Preferably, the stirring mechanism comprises a stirrer shaft and a paddle connected to the stirrer shaft, and the stirrer shaft passes through the first through hole and the second through hole and is fixed on the first sealing cover.

[0008] Preferably, the paddle comprises a first paddle, a second paddle and a third paddle, the first paddle, the second paddle and the third paddle are detachably connected to the stirrer shaft, the first paddle is arranged in the dissolving agent liquid distribution mechanism, and the second paddle and the third paddle are arranged at the lower end of the dissolving agent liquid distribution mechanism.

[0009] Preferably, the first paddle is a vortex blade, and the rotation of the first paddle drives the dissolving agent in the dissolving agent liquid distribution mechanism to be discharged from the liquid outlet hole.

[0010] Preferably, the temperature control layer comprises a temperature control medium inlet, a temperature control medium outlet and a temperature sensor, the temperature control medium inlet is arranged on the lower side of the side wall of the body, the temperature control medium outlet is oppositely arranged on the upper side of the side wall of the body, the temperature control layer circulates with a temperature control medium, the temperature control medium enters the temperature control layer through the temperature control medium inlet and then is discharged from the temperature control layer through the temperature control medium outlet.

[0011] Preferably, the temperature control medium is oil.

[0012] Preferably, the crystallization device is provided with a discharging mechanism at the bottom end, the discharging mechanism comprises a second sealing cover, the second sealing cover is communicated with a discharging port, the second sealing cover is provided with a third through hole, the second sealing cover is uniformly provided with a fifth limiting hole around the top end, the bolt passes through the second limiting hole and the fifth limiting hole to fix the second sealing cover on the body, and the temperature sensor is arranged in the third through hole.

[0013] Preferably, when the temperature sensor detects that the temperature in the body is increased to above the melting point of hydroxylamine salt, the temperature control medium in the temperature control layer is cooled to below the melting point of hydroxylamine salt to make the hydroxylamine salt precipitate.

[0014] Preferably, the crystallization device is fixed on a fixing mechanism, the fixing mechanism comprises fixing blocks and a support, the fixing blocks are symmetrically arranged on the outer side walls of the crystallization device, the support is symmetrically provided with limiting grooves relative to the fixing blocks, and the fixing blocks are clamped in the limiting grooves to fix the crystallization device on the support.

[0015] The beneficial effects of the utility model are that the stirring mechanism passes through the second through hole to stir in the dissolving agent liquid distribution mechanism and the body, the dissolving agent enters the crystallization device through the dissolving agent feed pipe, is stirred after the stirring mechanism and is then uniformly distributed to the body by the liquid distribution part, the hydroxylamine salt solution enters the body through the mother liquor feed pipe and is mixed with the dissolving agent to make the hydroxylamine salt crystallization separate out from the mother liquor, so that the crystallization device can uniformly distribute the dissolving liquid to the mother liquor, and the uniform crystalline substance is obtained by separation, and the problem of high local dissolving agent concentration is solved. BRIEF DESCRIPTION OF DRAWINGS

[0016] The utility model will be further described below in combination with the drawings and examples.

[0017] In the drawings: Figure 1 It is a front view of the hydroxylamine salt dissolving crystallization device of the utility model;

[0018] Figure 2 It is Figure 1 It is a top view of the crystallization device;

[0019] Figure 3 It is Figure 2 It is an A-A sectional view of the crystallization device

[0020] Figure 4 It is Figure 1 It is a partial three-dimensional sectional view of the crystallization device;

[0021] Figure 5 It is Figure 1 It is a structure schematic view of the dissolving agent liquid distribution mechanism of the crystallization device.

[0022] 1. Crystallization device; 100. Body; 101. First limiting hole; 102. Second limiting hole; 10. Feeding mechanism; 11. First sealing cover; 111. Solvent feed pipe; 112. First through hole; 113. Third limiting hole; 12. Solvent distribution mechanism; 121. Fixed part; 1211. Fourth limiting hole; 122. Liquid distribution part; 1221. Liquid outlet hole; 123. Second through hole; 13. Mother liquor feed pipe; 20. Stirring mechanism; 21. Stirring shaft; 22. Paddle; 221. First paddle; 222. Second paddle; 223. Third paddle; 30. Temperature control layer; 31. Temperature control medium inlet; 32. Temperature control medium outlet; 33. Temperature sensor; 40. Discharge mechanism; 41. Second sealing cover; 411. Discharge port; 412. Third through hole; 413. Fifth limiting hole; 50. Fixing mechanism; 51. Fixed block; 52. Bracket; 521. Limiting groove. DETAILED DESCRIPTION

[0023] In order to make the technical problems, technical solutions and beneficial effects of the present application clearer, the present application will be described in detail with reference to the drawings. The figure is a simplified schematic diagram, which only schematically illustrates the basic features of the present application, and therefore only shows the structures related to the present application. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0024] As shown in Figure 1 The present application provides a hydroxylamine salt solvent crystallization device 1 fixed on a fixing mechanism 50, which includes a body 100, a feeding mechanism 10 arranged at the top end of the body 100, a stirring mechanism 20 arranged in the body 100, a temperature control layer 30 arranged at the side of the body 100, and a discharge mechanism 40 arranged at the bottom end of the body 100.

[0025] As shown in Figures 2-5 The body 100 is a tank structure with an upper opening and a lower opening, and the body 100 is uniformly provided with first limiting holes 101 around the top end, and the body 100 is uniformly provided with second limiting holes 102 around the bottom end.

[0026] The feeding mechanism 10 includes a first sealing cover 11, a solvent distribution mechanism 12 arranged at the lower end of the first sealing cover 11, and a mother liquor feed pipe 13 communicated with the upper end side wall of the body 100.

[0027] The first sealing cover 11 is communicated with a solvent feed pipe 111, the bottom end of the first sealing cover 11 is uniformly provided with third limiting holes 113, and the first sealing cover 11 is provided with a first through hole 112 for solvent feeding.

[0028] The dissolving agent distributing mechanism 12 is a "bowl" structure, and the dissolving agent distributing mechanism 12 is divided into a fixed part 121 at the top and a distributing part 122 at the bottom,

[0029] The fixed part 121 is provided with a fourth limiting hole 1211, and the dissolving agent distributing mechanism 12 is fixed between the first sealing cover 11 and the body 100 through the third limiting hole 113, the fourth limiting hole 1211 and the first limiting hole 101.

[0030] The distributing part 122 is provided with a liquid outlet hole 1221 on the inclined side wall and the bottom surface, and the distributing part 122 is provided with a second through hole 123 at the bottom, and the stirring mechanism 20 passes through the second through hole 123 to stir in the dissolving agent distributing mechanism 12 and the body 100.

[0031] The stirring mechanism 20 includes a blender shaft 21 and a paddle 22 connected to the blender shaft 21, and the blender shaft 21 passes through the first through hole 112 and the second through hole 123 and is fixed to the first sealing cover 11.

[0032] The paddle 22 includes a first paddle 221, a second paddle 222 and a third paddle 223, and the first paddle 221, the second paddle 222 and the third paddle 223 are detachably connected to the blender shaft 21, the first paddle 221 is arranged in the dissolving agent distributing mechanism 12, and the second paddle 222 and the third paddle 223 are arranged at the lower end of the dissolving agent distributing mechanism 12.

[0033] The first paddle 221 is a vortex blade, and the first paddle 221 drives the dissolving agent in the dissolving agent distributing mechanism 12 to be discharged from the liquid outlet hole 1221.

[0034] The temperature control layer 30 includes a temperature control medium inlet 31, a temperature control medium outlet 32 and a temperature sensor 33, the temperature control medium inlet 31 is arranged at the lower side of the side wall of the body 100, the temperature control medium outlet 32 is arranged at the upper side of the side wall of the body 100, and the temperature control layer 30 circulates with a temperature control medium, the temperature control medium enters the temperature control layer 30 through the temperature control medium inlet 31, and then is discharged from the temperature control layer 30 through the temperature control medium outlet 32.

[0035] In this embodiment, the temperature control medium is oil.

[0036] The discharging mechanism 40 has a second sealing cover 41, the second sealing cover 41 is communicated with a discharging port 411, the second sealing cover 41 is provided with a third through hole 412, the second sealing cover 41 is uniformly provided with a fifth limiting hole 413 around the top end, the second sealing cover 41 is fixed on the body 100 through the second limiting hole 102 and the fifth limiting hole 413, and the third through hole 412 is internally provided with a temperature sensor 33.

[0037] The temperature sensor 33 detects that the temperature in the body 100 rises above the melting point of the hydroxylamine salt, and the temperature control medium in the temperature control layer 30 is cooled to below the melting point of the hydroxylamine salt to cause the hydroxylamine salt to precipitate.

[0038] The crystallization device 1 is fixed on the fixing mechanism 50, the fixing mechanism 50 comprises a fixing block 51 and a support 52, the fixing block 51 is symmetrically arranged on the outer side wall of the crystallization device 1, the support 52 is symmetrically provided with a limiting groove 521 relative to the fixing block 51, and the fixing block 51 is clamped in the limiting groove 521 to fix the crystallization device 1 on the support 52.

[0039] The working process of the hydroxylamine salt dissolution crystallization device 1 is as follows:

[0040] The dissolution agent enters the crystallization device 1 through the dissolution agent feeding pipe 111, is stirred by the stirring mechanism 20, and is then uniformly distributed into the body 100 through the liquid outlet holes 1221, and the hydroxylammonium salt solution enters the body 100 through the mother liquor feeding pipe 13 and is mixed with the dissolution agent to cause the hydroxylamine salt to precipitate from the mother liquor.

[0041] The temperature sensor 33 detects that the temperature in the body 100 rises above the melting point of the hydroxylamine salt, and the temperature control medium in the temperature control layer 30 is cooled to below the melting point of the hydroxylamine salt to cause the hydroxylamine salt to precipitate.

[0042] The hydroxylamine salt dissolution crystallization device 1 has the following beneficial effects:

[0043] 1. The dissolution agent liquid distribution mechanism 12 is provided with uniform liquid outlet holes 1221 on the inclined side, so that the dissolution agent is uniformly discharged from the liquid outlet holes 1221 and uniformly added into the mother liquor, and the problem of high local dissolution agent concentration is reduced.

[0044] 2. The first paddle 221 drives the dissolution agent to be fully stirred in the dissolution agent liquid distribution mechanism 12, and then the dissolution agent is discharged from the liquid outlet holes 1221 on the inclined side of the dissolution agent liquid distribution mechanism 12, so that the dissolution agent has a certain initial speed and is more easily mixed with the mother liquor.

[0045] It is to be noted that the terms used herein are only intended to describe specific embodiments and are not intended to limit the example embodiments according to the present application. As used herein, the singular form is intended to include the plural form, unless the context clearly indicates otherwise, and it should also be understood that, when the terms "comprise" and / or "include" are used in the specification, they indicate the presence of the features, steps, operations, devices, components and / or combinations thereof.

[0046] It should be noted that the terms "first", "second", and the like in the description and in the claims of the present application and in the above-described drawings are used only for distinguishing between similar objects and do not necessarily have to describe a specific order or sequence. It is to be understood that data thus designated can be interchanged, where appropriate, so that the embodiments of the present application described herein can be carried out in other than the order shown or described herein.

[0047] With the above ideal embodiments according to the present application as the inspiration, through the above description, relevant staff can make various changes and modifications without deviating from the scope of the present application. The technical scope of the present application is not limited to the content in the specification, and must be determined according to the scope of the claims.

Claims

1. A hydroxylamine salt solvus crystallization apparatus, characterized by: The crystallization device (1) comprises a body (100), a feeding mechanism (10) arranged at the top end of the body (100), a stirring mechanism (20) arranged in the body (100), a temperature control layer (30) arranged at the side of the body (100), and a discharging mechanism (40) arranged at the bottom end of the body (100), the feeding mechanism (10) comprises a first sealing cover (11) and a solvent distribution mechanism (12), the first sealing cover (11) is communicated with a solvent feeding pipe (111), the solvent distribution mechanism (12) is divided into a fixed part (121) at the top and a distribution part (122) at the bottom, the fixed part (121) is fixed between the first sealing cover (11) and the body (100) to fix the solvent distribution mechanism (12), the distribution part (122) is provided with liquid outlet holes (1221) on the inclined side wall and the bottom surface, the bottom of the distribution part (122) is provided with a second through hole (123), the upper end of the body (100) is communicated with a mother liquor feeding pipe (13), the stirring mechanism (20) passes through the second through hole (123) to stir in the solvent distribution mechanism (12) and the body (100), the solvent enters the crystallization device (1) from the solvent feeding pipe (111), is stirred by the stirring mechanism (20), and is then uniformly distributed into the body (100) by the distribution part (122), the hydroxylamine salt solution enters the body (100) from the mother liquor feeding pipe (13) to mix with the solvent, so that the hydroxylamine salt is precipitated from the mother liquor.

2. The hydroxylamine salt solvus crystallization apparatus of claim 1, wherein: The body (100) is uniformly provided with first limiting holes (101) around the top end, the body (100) is uniformly provided with second limiting holes (102) around the bottom end, the first sealing cover (11) is uniformly provided with third limiting holes (113) around the bottom end, the first sealing cover (11) is provided with a first through hole (112), the fixed part (121) is provided with a fourth limiting hole (1211), and the solvent distribution mechanism (12) is fixed between the first sealing cover (11) and the body (100) by bolts passing through the third limiting holes (113), the fourth limiting holes (1211) and the first limiting holes (101).

3. The hydroxylamine salt solvus crystallization apparatus of claim 2, wherein: The stirring mechanism (20) comprises a stirrer shaft (21) and a paddle (22) connected to the stirrer shaft (21), the stirrer shaft (21) passes through the first through hole (112) and the second through hole (123), and is fixed on the first sealing cover (11).

4. The hydroxylamine salt solvus crystallization apparatus of claim 3, wherein: The paddle (22) comprises a first paddle (221), a second paddle (222) and a third paddle (223), which are detachably connected to the blender shaft (21), the first paddle (221) is arranged in the dissolving agent liquid distribution mechanism (12), and the second paddle (222) and the third paddle (223) are arranged at the lower end of the dissolving agent liquid distribution mechanism (12).

5. The hydroxylamine salt solvus crystallization apparatus of claim 4, wherein: The first paddle (221) is a vortex blade, which drives the dissolving agent in the dissolving agent liquid distribution mechanism (12) to be discharged from the liquid outlet hole (1221).

6. The hydroxylamine salt solvus crystallization apparatus of claim 2, wherein: The temperature control layer (30) comprises a temperature control medium inlet (31), a temperature control medium outlet (32) and a temperature sensor (33), the temperature control medium inlet (31) is arranged on the lower side of the side wall of the body (100), the temperature control medium outlet (32) is arranged on the upper side of the side wall of the body (100) in a symmetrical manner, and the temperature control layer (30) is filled with temperature control medium, which enters the temperature control layer (30) through the temperature control medium inlet (31) and is discharged from the temperature control layer (30) through the temperature control medium outlet (32).

7. The hydroxylamine salt solvus crystallization apparatus of claim 6, wherein: The temperature control medium is oil.

8. The hydroxylamine salt solvus crystallization apparatus of claim 6, wherein: The crystallization device (1) is provided with a discharging mechanism (40) at the bottom end, the discharging mechanism (40) comprises a second sealing cover (41), the second sealing cover (41) is communicated with a discharging port (411), the second sealing cover (41) is provided with a third through hole (412), and the second sealing cover (41) is provided with fifth limiting holes (413) uniformly around the top end, bolts pass through the second limiting holes (102) and the fifth limiting holes (413) to fix the second sealing cover (41) on the body (100), and the third through hole (412) is internally provided with the temperature sensor (33).

9. The hydroxylamine salt solvus crystallization apparatus of claim 8, wherein: When the temperature sensor (33) detects that the temperature in the body (100) is higher than the melting point of hydroxylamine salt, the temperature control medium in the temperature control layer (30) is cooled to below the melting point of hydroxylamine salt to precipitate hydroxylamine salt.

10. The hydroxylamine salt solvus crystallization apparatus of claim 1, wherein: The crystallization device (1) is fixed on a fixing mechanism (50), the fixing mechanism (50) comprises fixing blocks (51) and supports (52), the fixing blocks (51) are symmetrically arranged on the outer side walls of the crystallization device (1), the supports (52) are symmetrically provided with limiting grooves (521) relative to the fixing blocks (51), and the fixing blocks (51) are clamped in the limiting grooves (521) to fix the crystallization device (1) on the supports (52).

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