CN216320003U - 3-amino-1, 2-propylene glycol continuous crude distillation system - Google Patents

3-amino-1, 2-propylene glycol continuous crude distillation system Download PDF

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CN216320003U
CN216320003U CN202122964202.6U CN202122964202U CN216320003U CN 216320003 U CN216320003 U CN 216320003U CN 202122964202 U CN202122964202 U CN 202122964202U CN 216320003 U CN216320003 U CN 216320003U
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马骅
孙晟中
贺满华
卢建林
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Inner Mongolia Saintchem Chemicals Co ltd
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Inner Mongolia Saintchem Chemicals Co ltd
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Abstract

The utility model discloses a 3-amino-1, 2-propylene glycol continuous crude distillation system which comprises a raw material storage tank, an ammonia water tank, a mixer, a primary reaction tower, a secondary reaction tower, a liquid alkali tank, an evaporator, a crystallization kettle, a centrifuge, a mother liquid temporary storage tank, a dehydration evaporation device and a crude product evaporation device, wherein an inlet of the mother liquid temporary storage tank is communicated with a liquid outlet of the centrifuge, an outlet of the mother liquid temporary storage tank is communicated with an inlet of the dehydration evaporation device, a mother liquid outlet of the dehydration evaporation device is communicated with an inlet of the crude product evaporation device, a steam outlet of the crude product evaporation device is communicated with an inlet of a crude product condenser, and an outlet of the crude product condenser is communicated with a crude product receiving tank. This scheme adopts dehydration evaporation plant, crude evaporation plant etc. to evaporate device thick in succession, has realized the operation of full flow serialization, does not need personnel to throw material, blowing and distillation operation, and it is many to have avoided the operation manual operation of current thick unit of evaporating, and problem that personnel intensity of labour is big has also avoided the heat transfer efficiency that intermittent distillation caused to hang down, problem that the energy consumption is high.

Description

3-amino-1, 2-propylene glycol continuous crude distillation system
The technical field is as follows:
the utility model relates to the field of 3-amino-1, 2-propylene glycol production, in particular to a continuous coarse distillation system for 3-amino-1, 2-propylene glycol.
Background art:
3-amino-1, 2-propanediol is an important fine chemical intermediate with CAS number of 616-30-8 and molecular formula of C3H9NO2The method is mainly used for producing X-CT nonionic contrast agent iohexol and synthesizing special materials, and is also used as a pesticide intermediate.
The synthesis process of 3-amino-1, 2-propanediol comprises five parts of hydrolysis, ammonolysis, crystallization, crude distillation and rectification, Chinese patent No. ZL201410383029.2 discloses a method for synthesizing 3-amino-1, 2-propanediol by using a continuous reaction device, which discloses a continuous reaction device comprising a mixer, a multi-stage tower type reaction tower, an evaporator, a crystallization kettle, a condenser, an absorption tower and a circulating pump, and documents describe hydrolysis, ammonolysis, crystallization and rectification processes, but do not describe the crude distillation process.
In the 3-amino-1, 2-propylene glycol synthesis process, after crystallization and centrifugal desalting, the obtained centrifugate contains conjugates of 3-amino-1, 2-propylene glycol, glycerol, 2-amino-1, 3-propylene glycol and 3-amino-1, 2-propylene glycol, the conjugates of glycerol and 3-amino-1, 2-propylene glycol need to be further subjected to crude distillation to distill out the conjugates of glycerol and 3-amino-1, 2-propylene glycol from the system, and then the crude product of the 3-amino-1, 2-propylene glycol obtained after the crude distillation is rectified to obtain a 3-amino-1, 2-propylene glycol product; in the industry, a kettle type intermittent distillation is adopted in a crude distillation unit in a 3-amino-1, 2-propanediol synthesis system, and the crude distillation unit is a simple distillation system consisting of a crude distillation kettle, a condenser, a receiving tank and a vacuum pump, wherein the operation process comprises the steps of feeding 3-amino-1, 2-propanediol mother liquor which is subjected to centrifugal treatment and is from a crystallization process into the crude distillation kettle through vacuum, starting a jacket of the crude distillation kettle for steam heating, dehydrating until the kettle temperature reaches 110 ℃, discharging dehydrated water from the receiving tank after the dehydration is finished, starting a Roots vacuum unit, and starting to receive a crude product of the 3-amino-1, 2-propanediol until an airless phase at the kettle temperature of 160 ℃ is obtained. The significant drawbacks of this process are: the rough steaming operation is performed by more manual operations, each rough steaming operation needs 1 person for full-time operation, and the labor intensity of the personnel is high. Meanwhile, the intermittent distillation has low heat transfer efficiency and high energy consumption. In the existing kettle type distillation, the feeding amount is 2.8 tons, and the distillation time of each kettle is 24 hours, namely the productivity is 82kg/h, and the productivity is lower.
The utility model has the following contents:
the utility model aims to provide a continuous rough distillation system for 3-amino-1, 2-propylene glycol, which solves the problems of high energy consumption, low yield and high labor intensity of personnel of the conventional rough distillation unit and solves the problems through continuous design.
The utility model is implemented by the following technical scheme: a3-amino-1, 2-propylene glycol continuous rough distillation system comprises a raw material storage tank, an ammonia water tank, a mixer, a primary reaction tower, a secondary reaction tower, a liquid caustic soda tank, an evaporator, a crystallization kettle and a centrifuge, wherein the raw material storage tank and the ammonia water tank are communicated with an inlet of the mixer through pipelines, an outlet of the mixer is communicated with an inlet of the primary reaction tower, an outlet of the primary reaction tower and the liquid caustic soda tank are communicated with an inlet of the secondary reaction tower through pipelines, an outlet of the secondary reaction tower is communicated with an inlet of the evaporator, a bottom outlet of the evaporator is communicated with the crystallization kettle, an outlet of the crystallization kettle is communicated with an inlet of the centrifuge, and a solid outlet of the centrifuge is communicated with a ground tank of the centrifuge;
it still includes mother liquor jar, dehydration evaporation plant, crude evaporation plant of keeping in, the import of mother liquor jar of keeping in with centrifuge's liquid outlet intercommunication, the export of mother liquor jar of keeping in with dehydration evaporation plant's import intercommunication, dehydration evaporation plant's mother liquor export with crude evaporation plant's import intercommunication, crude evaporation plant's steam outlet and crude condenser import intercommunication, crude condenser export and crude receiving tank intercommunication. The mother liquor after the dehydration passes through liquid level control valve control and controls certain flow and gets into crude product evaporation plant, evaporates out and gets into the crude product receiving tank after the condenser condensation of crude product, and the incomplete cauldron that gets into of cauldron continues the distillation, treats that the incomplete cauldron of cauldron evaporates the clean cauldron to when setting for the liquid level, and the incomplete discharge pump of chain cauldron squeezes into the incomplete collecting vessel of cauldron in.
Further, the system also comprises a heat exchanger, wherein a heat medium inlet of the heat exchanger is communicated with a steam outlet of the crude product evaporation device, a heat medium outlet of the heat exchanger is communicated with an inlet of the crude product condenser, a cold medium inlet of the heat exchanger is communicated with an outlet of the first-stage reaction tower, and a cold medium outlet of the heat exchanger is communicated with an inlet of the second-stage reaction tower.
Further, it still includes waste water condenser and waste water receiving tank, dehydration evaporation plant's steam outlet and waste water condenser's import intercommunication, waste water condenser's export with the import intercommunication of waste water receiving tank. After dehydration by the dehydration evaporation plant, the dehydrated wastewater enters the wastewater receiving tank after being condensed by the condensing system, and is pumped into the absorption tower through the wastewater discharge pump after being stored to a certain liquid level by the wastewater temporary storage tank to be used as water for the reaction system.
Further, the dehydration evaporation device is a falling film evaporator.
Further, the crude product evaporation device is a scraper evaporator.
The utility model has the advantages that: this scheme is through changing cauldron formula intermittent type distillation unit for dehydration evaporation plant, crude product evaporation plant etc. thick device of evaporating in succession, has realized full flow serialization operation, does not need personnel to throw material, blowing and distillation operation, and the operation manual operation who has avoided current thick unit of evaporating is many, and problem that personnel intensity of labour is big has also avoided the heat transfer efficiency who leads to the fact of intermittent type distillation low, problem that the energy consumption is high.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a continuous crude distillation system for 3-amino-1, 2-propylene glycol according to the present invention.
In the figure: raw materials storage tank 1, aqueous ammonia jar 2, blender 3, one-level reaction tower 4, second grade reaction tower 5, liquid caustic soda jar 6, evaporimeter 7, crystallization kettle 8, centrifuge 9, mother liquor jar 10 of keeping in, dehydration evaporation plant 11, crude evaporation plant 12, crude condenser 13, crude receiving tank 14, the incomplete cauldron of cauldron evaporates clean 15, the incomplete collecting vessel 16 of cauldron, heat exchanger 17, waste water condenser 18, waste water receiving tank 19, absorption tower 20, centrifuge geosyncline 21, waste water jar 22 of keeping in, crude storage tank 23.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A3-amino-1, 2-propanediol continuous rough distillation system comprises a raw material storage tank 1, an ammonia water tank 2, a mixer 3, a primary reaction tower 4, a secondary reaction tower 5, a liquid alkali tank 6, an evaporator 7, a crystallization kettle 8 and a centrifuge 9, wherein the raw material storage tank 1 and the ammonia water tank 2 are both communicated with the inlet of the mixer 3 through a pipeline, the outlet of the mixer 3 is communicated with the inlet of the primary reaction tower 4, the outlet of the primary reaction tower 4 and the liquid alkali tank 6 are both communicated with the inlet of the secondary reaction tower 5 through pipelines, the outlet of the secondary reaction tower 5 is communicated with the inlet of the evaporator 7, the outlet at the bottom of the evaporator 7 is communicated with the crystallization kettle 8, the outlet of the crystallization kettle 8 is communicated with the inlet of the centrifuge 9, and the solid outlet of the centrifuge 9 is communicated with a ground tank 21 of the centrifuge;
it still includes mother liquor jar 10, dehydration evaporation plant 11, crude evaporation plant 12 of keeping in, and the import of mother liquor jar 10 of keeping in communicates with centrifuge 9's liquid outlet, and the export of mother liquor jar 10 of keeping in communicates with dehydration evaporation plant 11's import, and dehydration evaporation plant 11's mother liquor export communicates with crude evaporation plant 12's import, and crude evaporation plant 12's steam outlet communicates with crude condenser 13 import, and crude condenser 13 export communicates with crude receiving tank 14. The dehydrated mother liquor enters a crude product evaporation device 12 by controlling a certain flow through a liquid level regulating valve, and the evaporated crude product is condensed by a condenser and then enters a crude product receiving tank 14; the kettle residue enters the kettle residue steaming and cleaning kettle 15 to continue distillation, and when the kettle residue steaming and cleaning kettle 15 reaches a set liquid level, the kettle residue is pumped into the kettle residue collecting barrel 16 by the chain kettle residue discharging pump.
In this embodiment, the dehydration evaporation device 11 is a falling film evaporator, and the crude product evaporation device 12 is a scraper evaporator.
The embodiment also comprises a heat exchanger 17, wherein a heat medium inlet of the heat exchanger 17 is communicated with a steam outlet of the crude product evaporation device 12, a heat medium outlet of the heat exchanger 17 is communicated with an inlet of the crude product condenser 13, a cold medium inlet of the heat exchanger 17 is communicated with an outlet of the first-stage reaction tower 4, and a cold medium outlet of the heat exchanger 17 is communicated with an inlet of the second-stage reaction tower 5.
The embodiment also comprises a waste water condenser 18 and a waste water receiving tank 19, wherein the steam outlet of the dehydration evaporation device 11 is communicated with the inlet of the waste water condenser 18, and the outlet of the waste water condenser 18 is communicated with the inlet of the waste water receiving tank 19. After being dehydrated by the dehydration evaporation device 11, the dehydrated wastewater is condensed by a condensing system and then enters the wastewater receiving tank 19, is stored to a certain liquid level by the wastewater temporary storage tank 22 and then is pumped into the absorption tower 20 by the wastewater discharge pump to be used as water for the reaction system.
In this scheme, equipment such as raw materials storage tank 1, aqueous ammonia jar 2, blender 3, one-level reaction tower 4, second grade reaction tower 5, liquid caustic soda jar 6, evaporimeter 7, crystallization kettle 8 and centrifuge 9 and connected mode are the same with in the ZL201410383029.2, and evaporimeter 7 has three grades altogether, and the gas that first two-stage evaporimeter 7 evaporated is sent into absorption tower 20 after the condensation and is absorbed the ammonia retrieval and utilization.
The working principle is as follows:
3-chlorine-1, 2-propylene glycol from a raw material storage tank 1 and ammonia water from an ammonia water tank 2 are fed into a mixer 3 to be mixed, the reaction starts in the mixing process, the mixture sequentially enters a first-stage reaction tower 4 and a second-stage reaction tower 5 to continue the reaction, liquid caustic soda is pumped into the second-stage reaction tower 5 from a liquid caustic soda tank 6 when the reaction mixture enters the second-stage reaction tower 5, the reaction mixture completely reacted in the second reaction tower enters an evaporator 7 from the part, close to the top, of the second-stage reaction tower 5, and most of surplus ammonia and part of water are evaporated from the reaction mixture through multi-stage evaporation and are absorbed and recycled; the materials after multi-stage evaporation mainly comprise 3-amino-1, 2-propylene glycol and salt, and also comprise a small amount of coupling products of glycerol, 2-amino-1, 3-propylene glycol and 3-amino-1, 2-propylene glycol, the materials enter a crystallization kettle 8 for cooling crystallization, and are filtered and desalted through a centrifuge 9;
the desalted centrifugate is sent into a mother liquor temporary storage tank 10 for temporary storage, then 3-amino-1, 2-propanediol mother liquor is quantitatively pumped into a dehydration evaporation device 11 through a mother liquor feeding pump and a flowmeter, materials enter from the top of the dehydration evaporation device 11, the dehydration evaporation device 11 is preheated through a steam heating system before feeding, after the 3-amino-1, 2-propanediol mother liquor enters the dehydration evaporation device 11, the evaporation temperature is controlled to be 90-100 ℃ through the linkage of the bottom temperature of an evaporator 7 and steam heating, gas phase enters a condenser from a gas phase port at the lower end of the evaporator 7, enters a waste water temporary storage tank 22 after condensation, liquid phase flows out from the bottom of the evaporator 7, enters from a side port of a crude product evaporation device 12, quantitatively enters the crude product evaporation device 12 through a liquid level regulating valve of the dehydration evaporation device 11 to complete crude product distillation, the temperature of the evaporator 7 is regulated through the linkage of a residual evaporation kettle 15 and a steam regulating valve of the crude product evaporation device 12, the temperature is controlled at 150 ℃ and 160 ℃, the gas phase enters the crude product condenser 13 from the gas phase port at the upper part of the crude product evaporation device 12, after condensation, the gas phase enters the crude product receiving tank 14 and is 3-amino-1, 2-propanediol crude product, after the liquid level of the crude product receiving tank 14 reaches the set liquid level high limit, the crude product receiving tank is placed into the crude product storage tank 23, and then rectification is carried out. And the liquid phase flows out from the bottom of the evaporator 7, enters the kettle residue steaming and cleaning kettle 15, continuously and completely distills 3-amino-1, 2-propylene glycol mother liquor which is not completely distilled, and when the kettle residue steaming and cleaning kettle 15 reaches the liquid level height, the kettle residue discharge pump is started in a chain manner to pump kettle residues into the kettle residue ton bucket.
In this embodiment, the gas phase obtained at the gas phase outlet at the upper part of the crude product evaporation device 12 is heated by the product of the first-stage reaction tower 4, and then enters the crude product condenser 13 for condensation, thereby effectively utilizing the heat energy thereof.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the utility model, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (5)

1. A3-amino-1, 2-propylene glycol continuous rough distillation system comprises a raw material storage tank, an ammonia water tank, a mixer, a primary reaction tower, a secondary reaction tower, a liquid caustic soda tank, an evaporator, a crystallization kettle and a centrifuge, wherein the raw material storage tank and the ammonia water tank are communicated with an inlet of the mixer through pipelines, an outlet of the mixer is communicated with an inlet of the primary reaction tower, an outlet of the primary reaction tower and the liquid caustic soda tank are communicated with an inlet of the secondary reaction tower through pipelines, an outlet of the secondary reaction tower is communicated with an inlet of the evaporator, a bottom outlet of the evaporator is communicated with the crystallization kettle, an outlet of the crystallization kettle is communicated with an inlet of the centrifuge, and a solid outlet of the centrifuge is communicated with a ground tank of the centrifuge;
its characterized in that, it still includes mother liquor jar, dehydration evaporation plant, crude product evaporation plant of keeping in, the import of mother liquor jar of keeping in with centrifuge's liquid outlet intercommunication, the export of mother liquor jar of keeping in with dehydration evaporation plant's import intercommunication, dehydration evaporation plant's mother liquor export with crude product evaporation plant's import intercommunication, crude product evaporation plant's steam outlet and crude product condenser import intercommunication, crude product condenser export and crude product receiving tank intercommunication.
2. The continuous crude distillation system for 3-amino-1, 2-propylene glycol according to claim 1, further comprising a heat exchanger, wherein a heat medium inlet of the heat exchanger is communicated with the steam outlet of the crude evaporation device, a heat medium outlet of the heat exchanger is communicated with an inlet of the crude condenser, a cold medium inlet of the heat exchanger is communicated with the outlet of the primary reaction tower, and a cold medium outlet of the heat exchanger is communicated with the inlet of the secondary reaction tower.
3. The continuous rough distillation system of 3-amino-1, 2-propylene glycol according to claim 1, further comprising a wastewater condenser and a wastewater receiving tank, wherein the steam outlet of the dehydration evaporation device is communicated with the inlet of the wastewater condenser, and the outlet of the wastewater condenser is communicated with the inlet of the wastewater receiving tank.
4. The continuous rough distillation system of 3-amino-1, 2-propanediol according to any one of claims 1 to 3, wherein the dehydration evaporation device is a falling film evaporator.
5. The continuous crude distillation system for 3-amino-1, 2-propanediol according to any one of claims 1 to 3, wherein the crude distillation device is a scraper evaporator.
CN202122964202.6U 2021-11-29 2021-11-29 3-amino-1, 2-propylene glycol continuous crude distillation system Active CN216320003U (en)

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CN202122964202.6U CN216320003U (en) 2021-11-29 2021-11-29 3-amino-1, 2-propylene glycol continuous crude distillation system

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Application Number Priority Date Filing Date Title
CN202122964202.6U CN216320003U (en) 2021-11-29 2021-11-29 3-amino-1, 2-propylene glycol continuous crude distillation system

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GR01 Patent grant
GR01 Patent grant
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of utility model: A Continuous Coarse Steam System for 3-Amino-1,2-propanediol

Effective date of registration: 20230303

Granted publication date: 20220419

Pledgee: Agricultural Bank of China Limited Alashan Left Banner Wusitai Sub-branch

Pledgor: INNER MONGOLIA SAINTCHEM CHEMICALS CO.,LTD.

Registration number: Y2023150000029

PE01 Entry into force of the registration of the contract for pledge of patent right