CN111013239A - Molecular sieve treater is used in purification of N-methyl pyrrolidone - Google Patents

Molecular sieve treater is used in purification of N-methyl pyrrolidone Download PDF

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Publication number
CN111013239A
CN111013239A CN201910252155.7A CN201910252155A CN111013239A CN 111013239 A CN111013239 A CN 111013239A CN 201910252155 A CN201910252155 A CN 201910252155A CN 111013239 A CN111013239 A CN 111013239A
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CN
China
Prior art keywords
molecular sieve
cylinder
flow guide
support cylinder
methylpyrrolidone
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Pending
Application number
CN201910252155.7A
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Chinese (zh)
Inventor
黄春锦
刘甫先
周伟
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Ganzhou Zhongneng Industrial Co ltd
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Ganzhou Zhongneng Industrial Co ltd
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Priority to CN201910252155.7A priority Critical patent/CN111013239A/en
Publication of CN111013239A publication Critical patent/CN111013239A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D207/00Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
    • C07D207/02Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D207/18Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
    • C07D207/22Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D207/24Oxygen or sulfur atoms
    • C07D207/262-Pyrrolidones
    • C07D207/2632-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
    • C07D207/2672-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom

Abstract

The invention discloses a molecular sieve processor for purifying N-methyl pyrrolidone, which belongs to the technical field of NMP purification treatment and solves the problems of low utilization rate and poor purification effect of a molecular sieve in the existing NMP treatment, and comprises a treatment tank body, a partition plate, a flow guide column, a support cylinder and a bearing cylinder, wherein the support cylinder is arranged above the flow guide column, the moisture content in the N-methyl pyrrolidone can be reduced through heating, a primary molecular sieve, a secondary molecular sieve and an active carbon layer are separated between the support cylinder and the bearing cylinder, the molecular sieve filters impurities carried in the primary molecular sieve and the active carbon layer, the impurities in the primary molecular sieve and the active carbon layer are adsorbed by active carbon particles in the active carbon layer, the concentration of heavy metal ions in the N-methyl pyrrolidone is effectively reduced, the molecular sieve and the active carbon layer are distributed in a cylindrical shape, the largest area of the molecular sieve is contacted with the N-methyl pyrrolidone to adsorb a, the effective utilization rate of the primary molecular sieve and the secondary molecular sieve is improved, and the practicability is improved.

Description

Molecular sieve treater is used in purification of N-methyl pyrrolidone
Technical Field
The invention relates to the technical field of NMP purification treatment, in particular to a molecular sieve treater for purifying N-methyl pyrrolidone.
Background
With the rapid development of scientific technology and the continuous application of lithium batteries, in the production of lithium batteries, because of the strong hygroscopicity of N-methylpyrrolidone (NMP), a galvanized iron barrel or a plastic barrel is generally adopted for transportation and storage, poor sealing is easy to occur, the moisture content is increased, and the grade of the NMP is reduced. The reagent grade NMP with the purity of more than or equal to 99.9 percent contains trace moisture of less than or equal to 0.01 percent, the electronic grade NMP with the purity of more than or equal to 99.9 percent contains trace moisture of less than or equal to 0.02 percent, and the common grade NMP with the purity of more than or equal to 99.8 percent contains trace moisture of less than or equal to 0.03 percent.
The dispersion of battery powder and the adhesiveness of PVDF are deteriorated by a trace amount of water in NMP, and the cycle performance and safety performance of the battery are affected by heavy metal ions (such as Fe, Na, Mg, Cu and the like) brought in the process of preparing NMP. The higher the grade of NMP used in the lithium ion battery batching process, the better the performance.
Chinese patent CN204689921U discloses an N-methylpyrrolidone purification device, which comprises a pretreatment tank, a first filtration tank, a second filtration tank and a finished product tank, wherein the bottom of the pretreatment tank is connected with the bottom of the first filtration tank, the top of the first filtration tank and the top of the second filtration tank, and the bottom of the second filtration tank and the top of the finished product tank through pipelines respectively, and the pretreatment tank is filled with a molecular sieve. Although the pretreatment tank is filled with the molecular sieve, the first filter tank and the second filter tank are filled with the activated carbon, the adsorption effect of the molecular sieve and the activated carbon and the multistage filtering effect of the activated carbon are utilized to reduce the concentration of trace moisture and heavy metal ions in the N-methylpyrrolidone, so that the purity of the N-methylpyrrolidone is improved.
However, the above-mentioned N-methylpyrrolidone purification apparatus has a complicated structure, requires a lot of equipment, and has a complicated process, and particularly, when N-methylpyrrolidone is dehumidified and purified, the efficiency is low, and the utilization rate of the molecular sieve is low due to the conventional arrangement. Therefore, it is desirable to provide a molecular sieve treater for purifying N-methylpyrrolidone, aiming at solving the above problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a molecular sieve processor for purifying N-methylpyrrolidone, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the utility model provides a molecular sieve treater is used in purification of N-methyl pyrrolidone, is including handling the jar body, baffle, water conservancy diversion post, a supporting cylinder and a bearing cylinder, and the internal portion of handling jar is equipped with the baffle, and establish to heating chamber and impurity chamber below the baffle, and the inlet pipe is connected to heating chamber bottom side, and the baffle middle part is connected with the water conservancy diversion post, and the water conservancy diversion post top is equipped with a supporting cylinder, and the supporting cylinder outside has set gradually elementary molecular sieve, second grade molecular sieve, filter screen section of thick bamboo, activated carbon layer and a bearing cylinder, and the internal chamber of sweeping of establishing of handling jar outside of bearing cylinder, the gas circuit that sweeps is connected at the top of the handling.
As a further scheme of the invention, a feed valve is arranged on the feed pipe, the feed pipe is communicated with the heating cavity, a heating pipe shell is arranged in the heating cavity, and a heating pipe is arranged in the heating pipe shell.
As a further scheme of the invention, the bottom of the heating cavity is communicated with the impurity cavity, and a sewage discharge outlet is arranged on the treatment tank body at the bottom of the impurity cavity.
As a further scheme of the invention, a sewage plug is arranged in the sewage outlet, the sewage plug is in threaded connection with the sewage outlet at the bottom of the treatment tank body, and a sealing ring is arranged between the sewage plug and the treatment tank body.
As a further scheme of the invention, a plurality of through flow guide holes are arranged in the flow guide column, the bottoms of the flow guide holes are communicated with the heating cavity, the tops of the flow guide holes are communicated with the compression cavity, the compression cavity is arranged in the support cylinder, and a plurality of uniform flow holes are arranged on the side wall of the support cylinder.
As a further scheme of the invention, a discharge valve is arranged on the discharge pipe, and the discharge pipe is communicated with the purging cavity.
As a further scheme of the invention, the primary molecular sieve and the secondary molecular sieve are molecular sieve particles arranged between the supporting cylinder and the filtering net cylinder, and are distributed between the supporting cylinder and the filtering net cylinder in a cylindrical shape.
As a further scheme of the invention, a cylinder opening at the bottom of the supporting cylinder is in threaded connection with a threaded opening between the flow guide column and the partition plate, and a primary molecular sieve, a secondary molecular sieve, a filter screen cylinder, an activated carbon layer and a bearing cylinder which are sequentially arranged outside the supporting cylinder are connected into a whole.
As a further scheme of the invention, the partition plates are equidistantly distributed on a plurality of flow guide columns, a supporting cylinder is arranged above each flow guide column, and a primary molecular sieve, a secondary molecular sieve, a filter screen cylinder, an activated carbon layer and a bearing cylinder are sequentially arranged outside each supporting cylinder.
As a further proposal of the invention, the sewage discharge pipe is connected with the treatment tank body and is welded at the bottom of the treatment tank body and communicated with the sewage discharge port at the bottom of the treatment tank body.
In conclusion, compared with the prior art, the invention has the following beneficial effects:
the molecular sieve processor for purifying the N-methyl pyrrolidone can reduce the moisture content in the N-methyl pyrrolidone by heating, separates a primary molecular sieve, a secondary molecular sieve and an activated carbon layer between a supporting cylinder and a bearing cylinder, filters impurities carried in the primary molecular sieve, and adsorbs the impurities through activated carbon particles in the activated carbon layer, so that the concentration of heavy metal ions in the N-methyl pyrrolidone is effectively reduced, the molecular sieve and the activated carbon layer are distributed in a cylindrical shape, and the largest area of the molecular sieve processor is contacted with the N-methyl pyrrolidone uniformly dispersed in a compression cavity through a plurality of uniform flow holes in the supporting cylinder, so that a large amount of impurities in the N-methyl pyrrolidone are adsorbed, the effective utilization rate of the primary molecular sieve and the secondary molecular sieve is improved, and the practicability is improved.
To more clearly illustrate the structural features and effects of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Drawings
Fig. 1 is a schematic structural diagram of the invention.
FIG. 2 is a schematic structural diagram of the distribution of molecular sieve and activated carbon layers between a support cylinder and a bearing cylinder in the invention.
Fig. 3 is a schematic structural view of the inventive flow guide column.
Reference numerals: 1-feeding pipe, 2-feeding valve, 3-heating chamber, 4-treatment tank body, 5-impurity chamber, 6-pollution discharge plug, 7-heating pipe shell, 8-heating pipe, 9-clapboard, 10-flow guide column, 11-flow guide hole, 12-discharging pipe, 13-discharging valve, 14-compression chamber, 15-support cylinder, 16-uniform flow hole, 17-primary molecular sieve, 18-secondary molecular sieve, 19-filter screen cylinder, 20-activated carbon layer, 21-bearing cylinder, 22-purging chamber and 23-purging gas circuit.
Detailed Description
The technical solution of the present invention is further described with reference to the accompanying drawings and specific embodiments.
Example 1
Referring to fig. 1 to 3, a molecular sieve processor for purifying N-methyl pyrrolidone comprises a processing tank 4, a partition plate 9, a flow guide column 10, a support cylinder 15 and a bearing cylinder 21, wherein the partition plate 9 is arranged in the processing tank 4, a heating cavity 3 and an impurity cavity 5 are arranged below the partition plate 9, the bottom side of the heating cavity 3 is connected with a feed pipe 1, the feed pipe 1 is provided with a feed valve 2, the feed pipe 1 is communicated with the heating cavity 3, a heating pipe shell 7 is arranged in the heating cavity 3, a heating pipe 8 is arranged in the heating pipe shell 7, and the water content in the N-methyl pyrrolidone can be reduced by heating; 3 bottoms in heating chamber intercommunication impurity chamber 5, be equipped with the drain on the treatment tank body 4 of 5 bottoms in impurity chamber, be equipped with blowdown stopper 6 in the drain, it is preferred, in this embodiment, be threaded connection between the drain of blowdown stopper 6 and treatment tank body 4 bottoms, and be equipped with the sealing washer between blowdown stopper 6 and the treatment tank body 4, when needs are to the impurity discharge of sediment in the impurity chamber 5, only need with blowdown stopper 6 from the treatment tank body 4 bottom twist get off can, be convenient for in time discharge the impurity of sediment in the impurity chamber 5.
The middle of the partition board 9 is connected with a flow guide column 10, a plurality of flow guide holes 11 which are communicated are arranged inside the flow guide column 10, the bottom of each flow guide hole 11 is communicated with the heating cavity 3, the top of each flow guide hole 11 is communicated with a compression cavity 14, the compression cavity 14 is arranged inside a support cylinder 15, a plurality of uniform flow holes 16 are arranged on the side wall of the support cylinder 15, a primary molecular sieve 17, a secondary molecular sieve 18, a filter screen cylinder 19, an activated carbon layer 20 and a bearing cylinder 21 are sequentially arranged outside the support cylinder 15, a purging cavity 22 is arranged inside a processing tank body 4 outside the bearing cylinder 21, a purging gas circuit 23 is connected with the top of the processing tank body 4, a discharge pipe 12 is connected onto the processing tank body 4 on the upper side of the partition board 9, a discharge valve 13 is arranged on the discharge pipe 12, the discharge pipe 12 is communicated with the purging cavity 22, and after the discharge valve, The N-methyl pyrrolidone filtered and purified by the filter screen cylinder 19 and the activated carbon layer 20 is discharged from the discharge pipe 12.
Further, in this embodiment, the primary molecular sieve 17 and the secondary molecular sieve 18 are molecular sieve particles disposed between the supporting cylinder 15 and the filtering net cylinder 19, and are cylindrically distributed between the supporting cylinder 15 and the filtering net cylinder 19, and the largest area of the primary molecular sieve 17 and the secondary molecular sieve 18 is in contact with the N-methylpyrrolidone uniformly dispersed in the compression chamber 14 through the plurality of flow equalizing holes 16 of the supporting cylinder 15, so as to adsorb a large amount of impurities therein, thereby improving the effective utilization rate of the primary molecular sieve 17 and the secondary molecular sieve 18, and improving the practicability.
Further, in this embodiment, a bottom opening of the support cylinder 15 is in threaded connection with a threaded opening between the diversion column 10 and the partition plate 9, the primary molecular sieve 17, the secondary molecular sieve 18, the filter screen cylinder 19, the activated carbon layer 20 and the bearing cylinder 21 which are sequentially arranged outside the support cylinder 15 are connected into a whole, and the support cylinder 15 can be assembled on the partition plate 9 only by screwing the support cylinder 15, so that the installation and the disassembly are convenient; preferably, the upper part of the treatment tank 4 is detachably assembled in two parts, and the support cylinder 15 can be conveniently taken out by opening the upper part of the treatment tank 4.
Further, in this embodiment, the partition plates 9 are equidistantly distributed on the plurality of flow guide columns 10, a support cylinder 15 is installed above each flow guide column 10, the primary molecular sieve 17, the secondary molecular sieve 18, the filter screen cylinder 19, the activated carbon layer 20 and the bearing cylinder 21 are sequentially arranged outside the support cylinder 15, and the N-methylpyrrolidone purification efficiency is improved by installing the plurality of components.
The sizes of the uniform flow holes 16, the primary molecular sieve 17, the secondary molecular sieve 18, the filter screen cylinder 19, the activated carbon layer 20 and the meshes or gaps on the bearing cylinder 21 on the supporting cylinder 15 gradually decrease, when the N-methylpyrrolidone is purified, the primary molecular sieve 17, the secondary molecular sieve 18 and the activated carbon layer 20 are separated between the supporting cylinder 15 and the bearing cylinder 21, the molecular sieve filters impurities carried in the N-methylpyrrolidone, and the activated carbon particles in the activated carbon layer 20 adsorb the impurities in the N-methylpyrrolidone, so that the concentration of heavy metal ions in the N-methylpyrrolidone is effectively reduced.
Further, the filter screen cylinder 19 is made of a 400-mesh stainless steel cylindrical filter screen.
Preferably, the purging gas circuit 23 is connected with a nitrogen generating device, the purging gas circuit 23 is introduced through nitrogen, the nitrogen is filled into the treatment tank 4, the N-methyl pyrrolidone is pressed into the discharge pipe 12 from the treatment tank 4 and is discharged, therefore, the feed valve 2 and the discharge valve 13 are closed, and the inside of the treatment tank 4 is conveniently purged after the blowdown plug 6 is opened.
Example 2
Referring to fig. 1 to 3, a molecular sieve treater for purifying N-methylpyrrolidone is obtained by replacing the drain plug 6 at the bottom of the treatment tank 4 with a drain pipe connected to the treatment tank 4, and the structure thereof is the same as that of example 1.
The blow off pipe welding is linked together in 4 bottoms of the processing jar body and with the drain of 4 bottoms of the processing jar body, and then conveniently with the direct blowdown pipe that emits into of impurity that deposits in the impurity chamber 5 of the processing jar body 4, makes things convenient for the discharge of impurity and handles its further collection.
In this embodiment, install the blowoff valve on the blow off pipe, the opening and close of blowoff valve is convenient for control the emission to impurity.
The technical principle of the present invention has been described above with reference to specific embodiments, which are merely preferred embodiments of the present invention. The protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. Other embodiments of the invention will occur to those skilled in the art without the exercise of inventive faculty, and such will fall within the scope of the invention.

Claims (10)

1. A molecular sieve treater for purifying N-methylpyrrolidone comprises a treatment tank body (4), a partition plate (9), a flow guide column (10), a support cylinder (15) and a bearing cylinder (21), wherein the partition plate (9) is arranged inside the treatment tank body (4), a heating cavity (3) and an impurity cavity (5) are arranged below the partition plate (9), the bottom side of the heating cavity (3) is connected with a feeding pipe (1), the molecular sieve treater is characterized in that the flow guide column (10) is connected to the middle of the partition plate (9), the support cylinder (15) is arranged above the flow guide column (10), a primary molecular sieve (17), a secondary molecular sieve (18), a filter screen cylinder (19), an activated carbon layer (20) and the bearing cylinder (21) are sequentially arranged outside the support cylinder (15), a purging cavity (22) is arranged in the treatment tank body (4) outside the bearing cylinder (21), and a purging gas circuit (23) is connected to the top, a discharge pipe (12) is connected to the treatment tank body (4) on the upper side of the clapboard (9).
2. The molecular sieve treater for N-methylpyrrolidone purification according to claim 1, characterized in that a feed valve (2) is installed on the feed pipe (1), the feed pipe (1) is communicated with the heating chamber (3), a heating pipe housing (7) is installed inside the heating chamber (3), and a heating pipe (8) is installed inside the heating pipe housing (7).
3. The molecular sieve treater for N-methylpyrrolidone purification according to claim 2, characterized in that the bottom of the heating chamber (3) is communicated with an impurity chamber (5), and a sewage drain is arranged on the treatment tank body (4) at the bottom of the impurity chamber (5).
4. The molecular sieve treater for N-methylpyrrolidone purification according to claim 3, characterized in that a sewage discharge plug (6) is arranged in the sewage discharge port, the sewage discharge plug (6) is in threaded connection with the sewage discharge port at the bottom of the treatment tank body (4), and a sealing ring is arranged between the sewage discharge plug (6) and the treatment tank body (4).
5. The molecular sieve treater for N-methylpyrrolidone purification according to claim 1, wherein a plurality of flow guide holes (11) are formed in the flow guide column (10), the bottoms of the flow guide holes (11) are communicated with the heating cavity (3), the tops of the flow guide holes (11) are communicated with the compression cavity (14), the compression cavity (14) is arranged in the support cylinder (15), and a plurality of uniform flow holes (16) are formed in the side wall of the support cylinder (15).
6. The molecular sieve treater for N-methylpyrrolidone purification according to claim 5, characterized in that a discharge valve (13) is installed on the discharge pipe (12), and the discharge pipe (12) is communicated with the purge chamber (22).
7. The molecular sieve treater for N-methylpyrrolidone purification according to claim 1, characterized in that the primary molecular sieve (17) and the secondary molecular sieve (18) are molecular sieve particles disposed between the support cylinder (15) and the filter screen cylinder (19), and are cylindrically distributed between the support cylinder (15) and the filter screen cylinder (19).
8. The molecular sieve treater for N-methylpyrrolidone purification according to claim 7, wherein a bottom opening of the support cylinder (15) is connected in a threaded opening between the flow guide column (10) and the partition plate (9), and the primary molecular sieve (17), the secondary molecular sieve (18), the filter screen cylinder (19), the activated carbon layer (20) and the bearing cylinder (21) which are sequentially arranged outside the support cylinder (15) are connected into a whole.
9. The molecular sieve treater for N-methylpyrrolidone purification according to claim 1, characterized in that the partition plates (9) are equidistantly distributed on a plurality of flow guide columns (10), a support cylinder (15) is installed above each flow guide column (10), and a primary molecular sieve (17), a secondary molecular sieve (18), a filter screen cylinder (19), an activated carbon layer (20) and a bearing cylinder (21) are sequentially arranged outside each support cylinder (15).
10. The molecular sieve treater for purifying N-methylpyrrolidone according to claim 3, characterized by a drain pipe connected to the treatment tank (4), the drain pipe is welded to the bottom of the treatment tank (4) and is communicated with a drain outlet at the bottom of the treatment tank (4).
CN201910252155.7A 2019-03-29 2019-03-29 Molecular sieve treater is used in purification of N-methyl pyrrolidone Pending CN111013239A (en)

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Application publication date: 20200417