CN211595470U - Device for purifying amino dodecanoic acid product - Google Patents
Device for purifying amino dodecanoic acid product Download PDFInfo
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- CN211595470U CN211595470U CN201922477141.3U CN201922477141U CN211595470U CN 211595470 U CN211595470 U CN 211595470U CN 201922477141 U CN201922477141 U CN 201922477141U CN 211595470 U CN211595470 U CN 211595470U
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Abstract
The utility model belongs to the technical field of fine chemical product, concretely relates to a device for purifying amino dodecanoic acid product. The utility model is used for purify device of amino dodecanoic acid product, including ground paste blender, intensification melting processor, adsorption bed, pre-crystallizer, foster brilliant ware, centrifuge, collection fluid reservoir, regeneration treatment fluid reservoir and water purification jar. The utility model reasonably designs the length-diameter ratio, the sectional area, the packing shape and the like of the pre-crystallizer, can form a proper amount of crystal nucleus during cooling, does not need to add a nucleating agent, avoids the introduction of impurity components, and simultaneously can avoid a crystallization sensitive area in which insoluble substances are separated out; when the dissolution condition of a slightly soluble or insoluble substance is changed, a large number of crystal nuclei are easily formed, the most conventional method is to add nucleation crystal seeds, the defect is to introduce new impurity components, and the process selects a special equipment structure and a special process method to avoid the problem.
Description
Technical Field
The utility model belongs to the technical field of fine chemical product, concretely relates to a device for purifying amino dodecanoic acid product.
Background
Nylon 12 is widely used, mainly for marine pipes, urban natural gas pipes, automobile fuel oil delivery pipes, automobile brake pipes, air-conditioning pipes, air-compression equipment hoses, industrial high-pressure hydraulic pipes, quick pipe joints, automobile anti-lock system spiral shafts, sliding parts of precision gears, cams and bearings, static electricity removing rollers of copiers, antistatic capacitors and IC chip guide rails, optical cable sheaths, transparent pipes, self-adhesive wire paint, noise elimination gears, sports shoe soles, cable buckles, tennis racket cable buckles and the like.
The amino dodecanoic acid is monomer for synthesizing nylon 12, and its synthesis process is limited at present, in which the ammoniation hydrogenation method has the characteristics of short synthesis process route and easily available raw material, but the prepared nylon 12 monomer a contains a small quantity of fatty acid derivative, and is insoluble in water, b contains a small quantity of salt (such as sodium chloride), and c has higher colour number (small quantity of coke and pigment), and its most-used separation method is that ① is boiled with large quantity of water, and is recrystallized, and its decolouring effect is poor, and its product loss is large, ② adopts ion exchange method to remove sodium chloride, and its decolouring effect is poor, and its product loss is also large, and ③ also has the advantages of[1]The method has the advantages of large product loss, complex process, high energy consumption and poor decolorization effect, ④ has an acetic acid recrystallization purification process disclosed by Japan company, and has obvious defects, on one hand, the acetic acid solvent circulation is large, the energy consumption is large, on the other hand, the operation environment is poor, the equipment corrosion is serious, the cost is high, and the product yield is low.
Non-patent documents: [1] jing Xiong et al, macromolecule communication, 1964.9 volume 6, 5 th phase, electrodialysis purification of sodium chloride containing 9-amino nonanoic acid.
Disclosure of Invention
Aiming at the defects existing in the prior art, the utility model provides a device for purifying an aminododecanoic acid product. The utility model reasonably designs the length-diameter ratio, the sectional area, the packing shape and the like of the pre-crystallizer, can form a proper amount of crystal nucleus during cooling, does not need to add a nucleating agent, avoids the introduction of impurity components, and simultaneously can avoid a crystallization sensitive area in which insoluble substances are separated out; when the dissolution condition of a slightly soluble or insoluble substance is changed, a large number of crystal nuclei are easily formed, the most conventional method is to add nucleation crystal seeds, the defect is to introduce new impurity components, and the process selects a special equipment structure and a special process method to avoid the problem.
In order to solve the technical problem, the utility model adopts the following technical scheme:
a device for purifying an aminododecanoic acid product, which comprises a slurry mixer, a heating melting processor, an adsorption bed and a pre-crystallizer, the device comprises a crystal growing device, a centrifugal machine, a liquid collecting tank, a regeneration treatment liquid tank and a water purifying tank, wherein an outlet of a slurry mixer is connected with an inlet of a heating melting processor, an outlet of the heating melting processor is connected with an inlet of an adsorption bed, an outlet of the adsorption bed is connected with an inlet of a pre-crystallizer, an outlet of the pre-crystallizer is connected with an inlet of the crystal growing device, an outlet of the crystal growing device is connected with a feed inlet of the centrifugal machine, a mother liquid outlet of the centrifugal machine is connected with an inlet of the liquid collecting tank, an outlet of the liquid collecting tank is connected with an inlet of the regeneration treatment liquid tank and an inlet of the slurry mixer, an inlet of the regeneration treatment liquid tank is connected with an outlet of the adsorption bed, a distillation outlet of the regeneration treatment.
The pre-crystallizer comprises a first pre-crystallizer and a second pre-crystallizer which are connected in series, stainless steel ring packing is filled in the first pre-crystallizer, the surface of the stainless steel ring packing is subjected to roughening treatment, and the surface roughness is
And a tetrafluoroethylene material with a smooth surface is filled in the second pre-crystallizer spiral tube.
Selecting rough surfaceThe stainless steel ring filler treated by chemical treatment utilizes the principle that liquid collides with a rough surface when flowing to generate energy absorption to form proper amount of crystal nuclei with the roughness of
The feed liquid discharged from the first pre-crystallizer obviously has no characteristics of slurry and turbid liquid any more, layering can be realized through proper settlement, the particle size is about 50-200 mu m, the roughness is too high, crystal residues exist on the surface, and the formation of too low crystal nuclei is not obvious; the sample is taken and tested on a laser particle size distribution tester, and the particle size of 98 percent is in the range of 100-200 mu m.
The tetrafluoroethylene material filled in the second pre-crystallizer is a triangular surface body, and the average geometric dimension of the tetrafluoroethylene material is less than 15mm multiplied by 15 mm.
The triangular face body filler mainly aims at forming holes so as to maintain proper void ratio, and the triangular face body tetrafluoroethylene material with smooth surface can change the fluid form and improve the mixing effect; the surface of the triangular surface is smooth, the flow velocity of the feed liquid is high, and new crystal nuclei are not easy to generate; because the surface of the triangular surface is smooth, the crystal is not easy to remain.
The slurry mixer is provided with a push type stirring device, and the length-diameter ratio of the slurry mixer is 2: 1, the rotating speed is 100-300 rpm/min, the thin and long structure is matched with a push type stirrer to be beneficial to liquid mixing, so that the consistency with the characteristics of the water phase slurry of the aminododecanoic acid can be ensured, and the consistency of the feeding concentration is maintained.
The slurry mixer comprises a first slurry mixer and a second slurry mixer which are connected in parallel, and a solid feeding hole, a liquid inlet and a gas inlet are formed in the top of the slurry mixer.
The heating melting processor is internally provided with a spiral pipe, the heating jacket is arranged outside the heating melting processor, the baffling is obvious, and the spiral pipe is thin and long, so that the heat and mass transfer effect is good.
The adsorption bed is internally provided with active carbon and comprises a first adsorption bed and a second adsorption bed which are connected in parallel and used in turn.
The activated carbon in the adsorption bed is wood carbon, the particle size is 5-20 meshes, the adsorption of the kalimeris indica is more than or equal to 150mg/g, and the specific surface area is more than or equal to 1500m2(iv)/g, pH 6-9.
The crystal growing device is provided with wide blade paddles (the diameter of an impeller is 400mm), the rotating speed is 15-20 rpm/min, and the crystal growing device is externally provided with a jacket and is connected with a cooling water system.
The wide paddle has large discharge capacity and strong axial driving force, and mainly plays a role of suspension, so that crystals in the feed liquid are uniformly suspended in the solution, the temperature of the feed liquid is consistent, and the crystals cannot be damaged and the growth of the crystals cannot be influenced because the paddle is slow and has no shearing function.
Compared with the prior art, the utility model has the advantages of it is following:
the utility model discloses use the active carbon adsorption bed to come the edulcoration purification, both can desorption impurity such as fatty acid derivative and organic acid, also can desorption color and luster, and the adsorption bed can be recycled repeatedly, has reduced the energy consumption, has reduced manufacturing cost, has reduced waste discharge.
The utility model reasonably designs the length-diameter ratio, the sectional area, the packing shape and the like of the pre-crystallizer, can form a proper amount of crystal nucleus during cooling, does not need to add a nucleating agent, avoids the introduction of impurity components, and simultaneously can avoid a crystallization sensitive area in which insoluble substances are separated out; when the dissolution condition of a slightly soluble or insoluble substance is changed, a large number of crystal nuclei are easily formed, the most conventional method is to add nucleation crystal seeds, the defect is to introduce new impurity components, and the process selects a special equipment structure and a special process method to avoid the problem.
To sum up, the utility model discloses but the serialization operation, the operation is stable, and is simple and convenient, and the reliability is high, and the quality is stable.
Drawings
Fig. 1 is a purification device and a process flow chart for purifying an aminododecanoic acid product according to the present invention.
Description of reference numerals: 1-slurry mixer; 2-a temperature-raising melting processor; 3-an adsorption bed; 4-a first pre-crystallizer; 5-a second pre-crystallizer; 6-crystal growing device; 7-a centrifuge; 8-liquid collection tank; 9-regeneration treatment liquid tank; 10-a water purification tank; 11-a circulating water pump; 12-a split water pump; 13-a regenerative water pump; 1A-a first slurry mixer; 1B-a second slurry mixer; 3A-a first adsorption bed; 3B-second adsorption bed.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings.
Example 1
As shown in figure 1, the device for purifying aminododecanoic acid product comprises a slurry mixer 1, a heating melting processor 2, an adsorption bed 3, a pre-crystallizer, a crystal growing device 6, a centrifuge 7, a liquid collecting tank 8, a regeneration processing liquid tank 9 and a water purifying tank 10, wherein an outlet 1-1 of the slurry mixer is connected with an inlet 2-1 of the heating melting processor, an outlet 2-2 of the heating melting processor is connected with an inlet 3-1 of the adsorption bed, an outlet 3-2 of the adsorption bed is connected with an inlet 4-1 of the first pre-crystallizer, an outlet 4-2 of the first pre-crystallizer is connected with an inlet 5-1 of the second pre-crystallizer, an outlet 5-2 of the second pre-crystallizer is connected with an inlet 6-1 of the crystal growing device, an outlet 6-2 of the crystal growing device is connected with a feed inlet 7-1 of the centrifuge, a mother liquid outlet 7-2 of the centrifuge is connected with an inlet 8-1, the outlet 8-2 of the liquid collecting tank is connected with the slurry mixer 1-2 through a circulating liquid pump 11 on one hand, and is connected with the inlet 9-1 of the regeneration treatment liquid tank through a diversion water pump 12 on the other hand, the outlet 9-3 of the regeneration treatment liquid tank is connected with the inlet 3-1 of the adsorption bed through a regeneration water pump 13, and is connected with the slurry mixer 1-2 through the regeneration water pump 13 at the same time, the inlet 9-2 of the regeneration treatment liquid tank is connected with the outlet 3-2 of the adsorption bed, the distillation outlet 9-4 of the regeneration treatment liquid tank is connected with the inlet 10-1 of the water purification tank, and the outlet 10-2 of the water purification tank is connected with the.
1 volume 1000L of ground paste blender is provided with impulse type agitating unit, its draw ratio 2: 1, the rotating speed is 100-300 rpm/min, the thin and long structure is matched with a push type stirrer to be beneficial to liquid mixing, so that the consistency with the characteristics of the water phase slurry of the aminododecanoic acid can be ensured, and the consistency of the feeding concentration is maintained.
Slurry mixer 1 includes parallelly connected first slurry mixer 1A and second slurry mixer 1B, and slurry mixer 1 top is provided with solid feed inlet, liquid inlet and air inlet.
The heating melting processor 2 is made of 316L stainless steel, the outer diameter is phi 125 multiplied by 1800mm, the pore size of the spiral pipe in the heating melting processor is phi 12 multiplied by 6000mm, and the heating jacket is arranged outside the heating melting processor.
The adsorption bed 3 is internally provided with activated carbon, the outer diameter is phi 200 multiplied by 1800mm, and the adsorption bed 3 comprises a first adsorption bed 3A and a second adsorption bed 3B which are connected in parallel and used in turn.
The activated carbon in the adsorption bed 3 is wood carbon, the particle size is 5-20 meshes, the adsorption of the kalimeris indica is more than or equal to 150mg/g, and the specific surface area is more than or equal to 1500m2(iv)/g, pH 6-9.
The resistance of the granular activated carbon bed layer is small, and the adsorption area is large; the optimal adsorption pH value of the granular activated carbon is 6-9, which is just consistent with the equilibrium pH value of the aminododecanoic acid solution of 6.9-7.6.
The pre-crystallizer comprises a first pre-crystallizer 4 and a second pre-crystallizer 5 which are connected in series and filled with stainless steel circular ring packing
The surface of the stainless steel ring packing is subjected to roughening treatment, and the surface roughness is
The inner diameter of the first pre-crystallizer 4 is phi 80 × 500mm, the inner diameter of the second pre-crystallizer 5 is phi 100 × 600mm, and a tetrafluoroethylene material with a smooth surface is filled in a spiral tube of the second pre-crystallizer 5.
The tetrafluoroethylene material filled in the second pre-crystallizer 5 is a triangular surface body, and the average geometric dimension of the tetrafluoroethylene material is less than 15mm multiplied by 15 mm.
The volume of the crystal growing device 6 is 1000L, the wide blade paddle (the diameter of the impeller is 400mm), the rotating speed is 15-20 rpm/min, and the cooling water system is connected with the jacket.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes made to the above embodiments according to the utility model all still belong to the protection scope of the technical scheme of the utility model.
Claims (9)
1. A device for purifying an aminododecanoic acid product is characterized by comprising a slurry mixer (1), a heating melting processor (2), an adsorption bed (3), a pre-crystallizer, a crystal growing device (6), a centrifugal machine (7), a liquid collecting tank (8), a regeneration processing liquid tank (9) and a water purifying tank (10), wherein an outlet of the slurry mixer (1) is connected with an inlet of the heating melting processor (2), an outlet of the heating melting processor (2) is connected with an inlet of the adsorption bed (3), an outlet of the adsorption bed (3) is connected with an inlet of the pre-crystallizer, an outlet of the pre-crystallizer is connected with an inlet of the crystal growing device (6), an outlet of the crystal growing device (6) is connected with a feed inlet of the centrifugal machine (7), a mother liquid outlet of the centrifugal machine (7) is connected with an inlet of the liquid collecting tank (8), an outlet of the liquid collecting tank (8) is connected with an inlet of the regeneration processing liquid tank (9, the inlet of the regeneration treatment liquid tank (9) is connected with the outlet of the adsorption bed (3), the distillation outlet of the regeneration treatment liquid tank (9) is connected with the inlet of the water purification tank (10), and the outlet of the regeneration treatment liquid tank (9) and the outlet of the water purification tank (10) are connected with the inlet of the adsorption bed (3) and the inlet of the slurry mixer (1).
2. The apparatus for purifying aminododecanoic acid product according to claim 1, wherein the pre-crystallizer comprises a first pre-crystallizer (4) and a second pre-crystallizer (5) connected in series, the first pre-crystallizer (4) is filled with stainless steel ring packing, the surface of the stainless steel ring packing is roughened, and the surface roughness is
And a tetrafluoroethylene material with a smooth surface is filled in the spiral tube of the second pre-crystallizer (5).
3. Apparatus for purifying an aminododecanoic acid product according to claim 2, wherein the tetrafluoroethylene material filled in the second pre-crystallizer (5) is a triangular body with average geometric dimensions < 15mm x 15 mm.
4. Apparatus for the purification of an aminododecanoic acid product according to claim 1, wherein the slurry mixer (1) is provided with a propeller type stirring device having a length to diameter ratio of 2: 1, the rotation speed is 100-300 rpm/min.
5. An apparatus for purifying an aminododecanoic acid product according to claim 1, wherein the slurry mixer (1) comprises a first slurry mixer (1A) and a second slurry mixer (1B) in parallel, and a solid feed port, a liquid inlet and a gas inlet are provided at the top of the slurry mixer (1).
6. The apparatus for purifying aminododecanoic acid product according to claim 1, wherein the temperature-rising melting processor (2) is provided with a spiral pipe and a heating jacket outside.
7. The apparatus for purifying aminododecanoic acid product according to claim 1, wherein the adsorption bed (3) contains activated carbon, and the adsorption bed (3) comprises a first adsorption bed (3A) and a second adsorption bed (3B) connected in parallel for alternate use.
8. The device for purifying aminododecanoic acid product according to claim 7, wherein the activated carbon in the adsorption bed (3) is wood charcoal, the particle size is 5-20 meshes, the adsorption of methylene blue is not less than 150mg/g, and the specific surface area is not less than 1500m2(iv)/g, pH 6-9.
9. The device for purifying aminododecanoic acid product according to claim 1, wherein the crystal growing device (6) is equipped with wide-blade paddle, rotating at 15-20 rpm/min, externally provided with jacket, and connected with cooling water system.
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| CN201922477141.3U CN211595470U (en) | 2019-12-31 | 2019-12-31 | Device for purifying amino dodecanoic acid product |
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| CN201922477141.3U CN211595470U (en) | 2019-12-31 | 2019-12-31 | Device for purifying amino dodecanoic acid product |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111004139A (en) * | 2019-12-31 | 2020-04-14 | 无锡殷达尼龙有限公司 | Green continuous process and device for purifying amino dodecanoic acid product |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111004139A (en) * | 2019-12-31 | 2020-04-14 | 无锡殷达尼龙有限公司 | Green continuous process and device for purifying amino dodecanoic acid product |
| CN111004139B (en) * | 2019-12-31 | 2023-10-31 | 无锡殷达尼龙有限公司 | Green continuous process and device for purifying aminododecanoic acid product |
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