CN209362157U - A kind of approximation VPSA is used to refine the molecular sieve device of low water content solvent - Google Patents

A kind of approximation VPSA is used to refine the molecular sieve device of low water content solvent Download PDF

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CN209362157U
CN209362157U CN201821934118.1U CN201821934118U CN209362157U CN 209362157 U CN209362157 U CN 209362157U CN 201821934118 U CN201821934118 U CN 201821934118U CN 209362157 U CN209362157 U CN 209362157U
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adsorption tower
import
molecular sieve
outlet
waste liquid
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熊春刚
杨震鸿
曹杨
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Guangzhou Hanzhi Blue Energy And Environmental Technology Co Ltd
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Guangzhou Hanzhi Blue Energy And Environmental Technology Co Ltd
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Abstract

The utility model discloses the molecular sieve devices that a kind of approximation VPSA is used to refine low water content solvent, including head tank, first adsorption tower, second adsorption tower, condenser, waste liquid tank, filter, products pot, constant-flux pump, heater and vacuum pump, the import of the discharge port and filter of head tank connects, the outlet of filter and the import of constant-flux pump connect, the outlet and the import of the first adsorption tower of constant-flux pump, the import of second adsorption tower connects, the outlet of first adsorption tower is connect with products pot import respectively with the outlet of the second adsorption tower, heater and the first adsorption tower, the connection of second adsorption tower, the waste liquid outlet of first adsorption tower is connect with the import of condenser respectively with the waste liquid outlet of the second adsorption tower, the outlet of condenser and the import of waste liquid tank connect, the upper end of waste liquid tank is controlled to a vacuum pump.The beneficial effect of the utility model be it is simple using route, at low cost, easily operated, take off that minor amount of water is high-efficient, and molecular sieve high-efficient regeneration and product yield are high.

Description

A kind of approximation VPSA is used to refine the molecular sieve device of low water content solvent
Technical field
The utility model relates to molecular sieve device field, in particular to a kind of approximation VPSA is for refining low water content solvent Molecular sieve device.
Background technique
What is used at present for solvent containing few (micro-) amount water abjection is traditional rectifying mode, but traditional rectificating method Need to consume the high pure solvent of too many energy consumption, especially higher boiling, recycling energy consumption is very big.One of Typical Representative, N- Methyl pyrrolidone (abbreviation NMP) is widely used in petrochemical industry, plastics industry, pesticide, dyestuff, material and lithium battery manufacture In industry.It is wherein widely used in lithium battery anode manufacturing process as solvent, the NMP as solvent utilizes hot-air by its vapour Condensing recovery after change.Water content is not more than 500ppm, sometimes even less than 200ppm or less to new NMP in solvent when in use.
Related waste liquid is directly met at the processing of Wei Fei company by lithium battery factory at present, and existing industrialization technology uses rectifying Tower is recycled, and the high-purity N MP solvent that this method obtains is used in mass production, is invested big energy consumption height, is unfavorable for few The recycling operation of NMP waste liquid is measured, simultaneously because NMP is separated from water ineffective, resulting waste water is severely exceeded, and also be easy to cause Environmental pollution, therefore it is badly in need of a kind of new method processing recycling nmp solvent of environmental protection and energy saving.
The method that NMP is recycled in patent CN106220548 A is that air-distillation recycling is carried out using two towers, and the first order is to steam Tower is evaporated, 90%NMP solution is obtained, wherein NMP to be purified, which enters back into the progress rectifying of product tower, obtains high-purity N MP, the essence purification Step recyclable device is complicated for this, takes up a large area, and energy consumption is high, is not suitable for a small amount of NMP processing to be purified
The active carbon and molecular sieve used described in patent CN101696182A carries out purification recycling NMP, entire technique mistake Journey seems simply, does not refer to or illustrate in the patent the regeneration of molecular sieve, and traditional regenerating molecular sieve mode It can not make to adsorb NMP and the molecular sieve of minor amount of water regenerates the requirement for reaching and reusing completely, so that molecular sieve absorption property It greatly reduces, molecular sieve is not appropriate for continuing adsorbing the requirement for reaching high pure solvent again at this time, thus generates useless solid. The nmp solvent for being adsorbed on molecular sieve surface simultaneously is easy carbonization at a temperature of conventional regeneration, and hinders the pass of regenerating molecular sieve Key problem, and this problem tends to ignore in regenerative process, the NMP ingredient of carbonization is dissolved by NMP, and is made to be purified Nmp solvent becomes black, and NMP would become hard to separate with carbonization component at this time, polluted can not reusing for NMP, generates a large amount of Waste liquid.Therefore above-mentioned patent seems simply, but the useless solid problem of brought additional waste liquid is not referred to and solved, whole Energy consumption and environmental issue make the method last decade of the patent all not obtain market approval.
United States Patent (USP) US4965370 is that alkali metal or alkali metal salt removal foreign metal ion are added in technical grade NMP, The NMP of high-purity is being obtained by continuous process rectifying, but this continuous rectification energy consumption is high, product quality is not easy to control, and And distillation process is difficult to control, and is unfavorable for industrialized production.
Therefore, in the prior art all there is how more quickly and efficiently the problem for the treatment of in situ recycling purification NMP.
Utility model content
The utility model provides a kind of approximation VPSA molecular sieve device for being used to refine low water content solvent, can solve State the problem of proposing in background technique.
The utility model provides the molecular sieve device that a kind of approximation VPSA is used to refine low water content solvent, including raw material Tank, the first adsorption tower, the second adsorption tower, condenser, waste liquid tank, filter, products pot, constant-flux pump, heater, feed opening and true The discharge port of sky pump, the head tank is connect by pipeline with the import of the filter, and the outlet of the filter passes through pipe Road is connect with the import of the constant-flux pump, and the outlet of the constant-flux pump passes through the import of pipeline and first adsorption tower, described The import of second adsorption tower connects, the outlet of first adsorption tower and the outlet of second adsorption tower pass through respectively pipeline with The products pot import connection, the heater is connect by pipeline with first adsorption tower, second adsorption tower, described The waste liquid outlet of the waste liquid outlet of first adsorption tower and second adsorption tower passes through the import of pipeline Yu the condenser respectively The outlet of connection, the condenser is connect by pipeline with the import of the waste liquid tank, and the upper end of the waste liquid tank passes through pipeline It is connect with the vacuum pump.
Preferably, the upper end of the head tank is connected with the feed opening for adding raw material.
Preferably, the interior specification with second adsorption tower of first adsorption tower is 50 X of Φ, 500 adsorption tower, in It is provided with spherical or strip the molecular sieve of 2-3mm, the molecular sieve is 3A or 4A model.
Preferably, the import of the heater is also connected with conveying air pump, the import of the conveying air pump is connected with nitrogen Tank.
A kind of approximation VPSA provided by the utility model is used to refine the molecular sieve device of low water content solvent, to molecule into The effective regeneration of row, reaches and adsorbs requirement again, which uses route simple, at low cost, easily operated, takes off micro Water is high-efficient, and molecular sieve high-efficient regeneration, product yield is high, and industrialization is easier to realize.
Detailed description of the invention
Fig. 1 is the molecular sieve device signal that a kind of approximation VPSA provided by the utility model is used to refine low water content solvent Figure.
Description of symbols: 1- head tank;The first adsorption tower of 2-;The second adsorption tower of 3-;4- condenser;5- waste liquid tank;6- Filter;7- products pot;8- constant-flux pump;9- heater;10- feed opening;11- vacuum pump.
Specific embodiment
With reference to the accompanying drawing, a specific embodiment of the utility model is described in detail, it is to be understood that this The protection scope of utility model is not limited by the specific implementation.
As shown in Figure 1, a kind of approximation VPSA provided by the embodiment of the utility model is used to refine point of low water content solvent Sub- screen device, including head tank 1, the first adsorption tower 2, the second adsorption tower 3, condenser 4, waste liquid tank 5, filter 6, products pot 7, The discharge port of constant-flux pump 8, heater 9, feed opening 10 and vacuum pump 11, the head tank 1 passes through pipeline and the filter 6 The outlet of import connection, the filter 6 is connect by pipeline with the import of the constant-flux pump 8, and the outlet of the constant-flux pump 8 is logical It crosses pipeline to connect with the import of first adsorption tower 2, the import of second adsorption tower 3, the outlet of first adsorption tower 2 Pass through pipeline respectively with the outlet of second adsorption tower 3 to connect with 7 import of products pot, the heater 9 passes through pipeline It is connect with first adsorption tower 2, second adsorption tower 3, the waste liquid outlet of first adsorption tower 2 and second absorption The waste liquid outlet of tower 3 passes through pipeline respectively and connect with the import of the condenser 4, the outlet of the condenser 4 by pipeline with The import of the waste liquid tank 5 connects, and the upper end of the waste liquid tank 5 is connect by pipeline with the vacuum pump 11.
The upper end of the head tank 1 is connected with the feed opening 10 for adding raw material.
In first adsorption tower 2 and the specification of second adsorption tower 3 is 50 X of Φ, 500 adsorption tower, is inside all provided with It is equipped with spherical or strip the molecular sieve of 2-3mm, the molecular sieve is 3A or 4A model.
The import of the heater 9 is also connected with conveying air pump, and the import of the conveying air pump is connected with nitrogen gas tank.
Regenerating molecular sieve is realized using the molecular sieve device that a kind of above-mentioned approximation VPSA is used to refine low water content solvent Embodiment are as follows:
Case study on implementation 1
N-Methyl pyrrolidone 2L to be purified is injected into head tank 1, water content 0.5% is 50 X of Φ by specification 500 the first adsorption tower 2, the second adsorption tower 3, molecular sieve are the spherical or strip of Φ 2-3mm, and molecular sieve selects 3A or 4A type Number, NMP to be purified passes through filter 6, the first adsorption tower 2, the second adsorption tower 3 that deliver by constant-flux pump 8, flow control For 0.6L/h, product enters products pot 7 after absorption, and whole system closes drying, product yield 97%.
Regenerating molecular sieve process is as follows in first adsorption tower 2, the second adsorption tower 3, first with nitrogen by molecular sieve surface nitrogen Drying prevents the NMP carbonization for being adsorbed on molecular sieve surface, influences absorption and the regeneration effect of molecular sieve.Nitrogen is heated to 70 DEG C, It is vacuumized in the first adsorption tower 2 simultaneously, the second adsorption tower 3, vacuum degree 50KPa, after purging 1 hour, molecular sieve surface NMP is taken out of by nitrogen, and waste nitrogen gas enters waste liquid tank by cooling collect of normal-temperature water;The temperature of nitrogen is risen to 300 DEG C again, then Raw 3h, regenerating molecular sieve finishes at this time.
Case study on implementation 2
N-Methyl pyrrolidone 2L to be purified is injected into head tank 1, water content 1% is 50 X 500 of Φ by specification The first adsorption tower 2, the second adsorption tower 3, molecular sieve be Φ 2-3mm spherical or strip, molecular sieve select 3A or 4A model, The first adsorption tower 2, the second adsorption tower 3 that NMP to be purified passes through filter 6, delivers by constant-flux pump 8, flow control are 0.5L/h, product enters products pot 7 after absorption, and whole system closes drying, product yield 96%.
Regenerating molecular sieve process is as follows in first adsorption tower 2, the second adsorption tower 3, first with nitrogen by molecular sieve surface nitrogen Drying prevents the NMP carbonization for being adsorbed on molecular sieve surface, influences absorption and the regeneration effect of molecular sieve.Nitrogen is heated to 90 DEG C, It is vacuumized in the first adsorption tower 2 simultaneously, the second adsorption tower 3, vacuum degree 70KPa, purging is after 1.5 hours, molecular sieve surface NMP taken out of by nitrogen, waste nitrogen gas enters waste liquid tank by cooling collect of normal-temperature water;The temperature of nitrogen is risen to 350 DEG C again, 3h is regenerated, regenerating molecular sieve finishes at this time.
Case study on implementation 3
N-Methyl pyrrolidone 2L to be purified is injected into head tank 1, water content 0.3% is 50 X of Φ by specification 500 the first adsorption tower 2, the second adsorption tower 3, molecular sieve are the spherical or strip of Φ 2-3mm, and molecular sieve selects 3A or 4A type Number, NMP to be purified passes through filter 6, the first adsorption tower 2, the second adsorption tower 3 that deliver by constant-flux pump 8, flow control For 1L/h, product enters products pot 7 after absorption, and whole system closes drying, product yield 98%.
Regenerating molecular sieve process is as follows in first adsorption tower 2, the second adsorption tower 3, first with nitrogen by molecular sieve surface nitrogen Drying prevents the NMP carbonization for being adsorbed on molecular sieve surface, influences absorption and the regeneration effect of molecular sieve.Nitrogen is heated to 100 DEG C, at the same the first adsorption tower 2, vacuumize in the second adsorption tower 3, vacuum degree 80KPa, purging is after 2 hours, molecular sieve surface NMP taken out of by nitrogen, waste nitrogen gas enters waste liquid tank by cooling collect of normal-temperature water;The temperature of nitrogen is risen to 400 DEG C again, 3h is regenerated, regenerating molecular sieve finishes at this time.
A kind of approximation VPSA provided by the utility model is used to refine the molecular sieve device of low water content solvent, to molecule into The effective regeneration of row, reaches and adsorbs requirement again, which uses route simple, at low cost, easily operated, takes off micro Water is high-efficient, and molecular sieve high-efficient regeneration, product yield is high, and industrialization is easier to realize.
Disclosed above is only specific embodiment of the utility model, and still, the utility model embodiment is not limited to This, the changes that any person skilled in the art can think of should all fall into the protection scope of the utility model.

Claims (4)

1. a kind of approximation VPSA is used to refine the molecular sieve device of low water content solvent, it is characterised in that: including head tank (1), First adsorption tower (2), the second adsorption tower (3), condenser (4), waste liquid tank (5), filter (6), products pot (7), constant-flux pump (8), the discharge port of heater (9), feed opening (10) and vacuum pump (11), the head tank (1) passes through pipeline and the filtering The import of device (6) connects, and the outlet of the filter (6) is connect by pipeline with the import of the constant-flux pump (8), the advection The outlet of pump (8) is connect by pipeline with the import of the import of first adsorption tower (2), second adsorption tower (3), described The outlet of first adsorption tower (2) and the outlet of second adsorption tower (3) pass through pipeline respectively and the products pot (7) import connects It connects, the heater (9) is connect by pipeline with first adsorption tower (2), second adsorption tower (3), and described first inhales The waste liquid outlet of the waste liquid outlet of attached tower (2) and second adsorption tower (3) pass through respectively pipeline and the condenser (4) into Mouthful connection, the outlet of the condenser (4) are connect by pipeline with the import of the waste liquid tank (5), the waste liquid tank (5) it is upper End is connect by pipeline with the vacuum pump (11).
2. a kind of approximation VPSA as described in claim 1 is used to refine the molecular sieve device of low water content solvent, feature exists In the upper end of the head tank (1) is connected with the feed opening (10) for adding raw material.
3. a kind of approximation VPSA as described in claim 1 is used to refine the molecular sieve device of low water content solvent, feature exists In in first adsorption tower (2) and the specification of second adsorption tower (3) is 50 X of Φ, 500 adsorption tower, is inside respectively provided with There is spherical or strip the molecular sieve of 2-3mm, the molecular sieve is 3A or 4A model.
4. a kind of approximation VPSA as described in claim 1 is used to refine the molecular sieve device of low water content solvent, feature exists In the import of the heater (9) is also connected with conveying air pump, and the import of the conveying air pump is connected with nitrogen gas tank.
CN201821934118.1U 2018-11-22 2018-11-22 A kind of approximation VPSA is used to refine the molecular sieve device of low water content solvent Active CN209362157U (en)

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