CN112225680A - Organic solvent purification method and device - Google Patents
Organic solvent purification method and device Download PDFInfo
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- CN112225680A CN112225680A CN201910638086.3A CN201910638086A CN112225680A CN 112225680 A CN112225680 A CN 112225680A CN 201910638086 A CN201910638086 A CN 201910638086A CN 112225680 A CN112225680 A CN 112225680A
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- 239000003960 organic solvent Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000000746 purification Methods 0.000 title claims abstract description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 132
- 239000007788 liquid Substances 0.000 claims abstract description 49
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims description 19
- 238000005192 partition Methods 0.000 claims description 15
- 238000001704 evaporation Methods 0.000 claims description 12
- 239000002699 waste material Substances 0.000 claims description 11
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000003672 processing method Methods 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 11
- 229920000049 Carbon (fiber) Polymers 0.000 description 9
- 239000004917 carbon fiber Substances 0.000 description 9
- 208000005156 Dehydration Diseases 0.000 description 8
- 230000018044 dehydration Effects 0.000 description 8
- 238000006297 dehydration reaction Methods 0.000 description 8
- 238000004821 distillation Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000007670 refining Methods 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 4
- 238000007380 fibre production Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 239000012808 vapor phase Substances 0.000 description 4
- 239000012043 crude product Substances 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 150000003462 sulfoxides Chemical class 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000009270 solid waste treatment Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method and a device for purifying an organic solvent, which mainly solve the problems of longer process flow, higher equipment investment and energy consumption in the prior art, and adopts an organic solvent purification device which comprises a rectifying tower (1), a first reboiler (2), a second reboiler (3), a first condenser (6) and a second condenser (7); the device is characterized in that at least a first clapboard (8) and a second clapboard (9) are arranged in the rectifying tower (1), a first channel is formed between the first clapboard and the tower wall, and a first gas-liquid contact internal part (10) is arranged in the first channel; a second channel is formed between the first clapboard and the second clapboard, and a second gas-liquid contact internal part (11) is arranged in the second channel; the third channel is formed between the second clapboard and the tower wall, and the third gas-liquid contact internal part (12) is arranged in the third channel, so that the problem is better solved, and the method can be used for the recovery and treatment industrial application of organic solvents, particularly dimethyl sulfoxide.
Description
Technical Field
The invention relates to a method and a device for recovering and purifying an organic solvent, in particular to a method and a device for purifying dimethyl sulfoxide.
Technical Field
Solvent recovery is an important production unit within carbon fiber plants. Dimethyl sulfoxide recycled by the industrial device accounts for more than 90% of the total amount of the solvent demand, and directly influences the production cost, so the PAN protofilament device must be matched with a solvent recovery facility.
The solvent recovery usually adopts the vacuum rectification operation, the energy consumption is high, and the consumption of heating steam and circulating cooling water of the unit is far higher than that of other units, so the method is also an important link for saving energy and reducing consumption in the carbon fiber device. According to the production practice of carbon fibers, dimethyl sulfoxide suitable for the polymerization production of carbon fibers has higher requirements on reducing impurities, transmittance and metal ions.
In industrial production, the dimethyl sulfoxide solvent recovery mostly adopts a multi-tower continuous rectification process, and the process is divided into four working procedures of pretreatment, dehydration, refining and post-treatment and is provided with an auxiliary vacuum system. The main purposes of pretreatment are polymer removal and deacidification; the dehydration unit is mainly used for separating water from the dimethyl sulfoxide waste liquid, the dimethyl sulfoxide content in water is required to be far lower than 1%, and the industrial discharge requirement is met; the refining unit is mainly used for obtaining high-concentration dimethyl sulfoxide as a final product, and the requirement of solvent recycling in the carbon fiber production process is met.
Chinese patent CN107459472 proposes to remove the polymer first, the treated raw material is dehydrated by vacuum rectification, and the dehydrated material is subjected to vacuum rectification to obtain a high-concentration dimethyl sulfoxide product.
Chinese patent CN102225904 provides a device for recovering and refining dimethyl sulfoxide and a separation method thereof, comprising a first-stage dehydration tower, a wiped film evaporator, a primary distillation intermediate tank, a second-stage dehydration tower and a DMSO refining tower, wherein the first-stage dehydration tower is connected with the primary distillation intermediate tank, the wiped film evaporator is connected with the primary distillation intermediate tank, and then the second-stage dehydration tower and the DMSO refining tower are sequentially connected. The dimethyl sulfoxide raw material is divided into two strands, the low-concentration DMSO raw material does not contain high polymers, the DMSO content is 2.0% -15.0%, the dimethyl sulfoxide raw material directly enters a first-stage dehydration tower, and most of water in the raw material is removed; the high-concentration DMSO raw material contains high polymer, the DMSO content is 22.0-50.0%, the high polymer is removed by a wiped film evaporator, then the high polymer and the dehydrated low-concentration raw material enter a secondary dehydration tower together, and the dehydrated raw material is subjected to reduced pressure rectification again to obtain the high-concentration dimethyl sulfoxide.
Chinese patent 104119256 proposes a method for purifying dimethyl sulfoxide, which comprises the steps of: feeding the raw material containing dimethyl sulfoxide into a first evaporator for heating, carrying out vapor-liquid separation after partial evaporation, and feeding the obtained vapor phase into a rectifying tower; inputting the obtained liquid phase into a second evaporator for heating, performing vapor-liquid separation after partial evaporation, inputting the obtained vapor phase into a rectifying tower, and inputting the obtained liquid phase into a wiped film evaporator; collecting a dimethyl sulfoxide crude product at the tower bottom of the rectifying tower, inputting the dimethyl sulfoxide crude product into a third evaporator for heating, carrying out vapor-liquid separation after partial evaporation, inputting the obtained liquid phase into a wiped film evaporator, and returning the obtained vapor phase to the rectifying tower as a feed; and heating the third evaporator, partially evaporating, separating vapor from liquid, and returning the vapor phase obtained by vapor-liquid separation to the first evaporator as a heating medium, and condensing to obtain purified dimethyl sulfoxide.
Chinese patent CN104891591B proposes a method for recycling dimethyl sulfoxide, which comprises the steps of enabling waste water containing 0.5-1% of acrylonitrile and 1-5% of dimethyl sulfoxide to enter an acrylonitrile removing tower, firstly removing acrylonitrile in the water under reduced pressure for quality separation treatment, removing water from the waste water in the tower bottom through a dimethyl sulfoxide concentrating tower and a crude product tower under reduced pressure to enable the content of the dimethyl sulfoxide to reach 99%, and then performing reduced pressure rectification through a refining tower to obtain the dimethyl sulfoxide with the purity of more than 99.97%.
Chinese patent CN106674066 proposes a dimethyl sulfoxide purification method, which comprises the following steps: 1) deacidifying and dewatering; 2) carrying out reduced pressure distillation; 3) carrying out first melting crystallization; 4) and (4) carrying out second melting crystallization. The purity of the dimethyl sulfoxide obtained by the steps is more than or equal to 99.99 percent, and the yield is higher by about 85 percent.
The above patents have common problems of long process flow and high energy consumption.
Chinese patent CN107459472 proposes to obtain chromatographic grade dimethyl sulfoxide by using the following steps: (1) mixing and stirring raw materials of dimethyl sulfoxide and activated alumina, (2) distilling the adsorbed dimethyl sulfoxide and calcium hydride under reduced pressure, wherein the distillation pressure is 12mmHg, and the distillation temperature is about 70-90 ℃, so that the dimethyl sulfoxide is dehydrated and dried; (3) and storing the distillate in a storage tank filled with a 4A molecular sieve to obtain the chromatographic grade dimethyl sulfoxide. Obviously, the technology is used for preparing chromatographic grade dimethyl sulfoxide on the basis of obtaining high-concentration dimethyl sulfoxide, and is not suitable for recovering dimethyl sulfoxide waste liquid in carbon fiber production.
Chinese patent CN 107362568 proposes a solvent recovery method in carbon fiber production, which utilizes a vacuum rectification tower, wherein the upper section in the tower is filled with filler, and the lower section is a tower plate. Obtaining dimethyl sulfoxide products after decompression and rectification. It is clear that it is possible to obtain high concentrations of dimethyl sulfoxide from the bottom of the column obtained by means of a vacuum distillation column, which have the disadvantages of metal ion content and color intensity, and of the fact that heavy-end impurities cannot be removed.
Chinese patent CN1887864 proposes that metal ions in dimethyl sulfoxide are removed by using the principle of ion exchange, iron ions in sulfoxide are removed by using macroporous weakly-basic anion exchange resin, and calcium, magnesium, sodium and potassium ions in dimethyl sulfoxide are removed by using macroporous strongly-acidic cation exchange resin. Although the method can remove metal ions in sulfoxide, the influence of acrylonitrile polymer on the adsorption process is not considered, and the method is limited by the adsorption capacity, so that solid waste is inevitably generated, and the solid waste treatment is easy to cause secondary pollution.
Disclosure of Invention
The invention provides an organic solvent purification treatment device, which has the advantages of simple equipment process, low energy consumption and high removal efficiency.
The second technical problem to be solved by the invention is that although the prior art has a process for recycling the organic solvent waste liquid, particularly the dimethyl sulfoxide waste liquid, the process flow is longer, and the equipment investment and energy consumption are higher.
In order to solve one of the above technical problems, the technical scheme adopted by the invention is as follows: an organic solvent purification device comprises a rectifying tower 1, a first reboiler 2, a second reboiler 3, a first condenser 6 and a second condenser 7; at least a first clapboard 8 and a second clapboard 9 are arranged in the rectifying tower 1, a first channel is formed between the first clapboard and the tower wall, and a first gas-liquid contact internal part 10 is arranged in the first channel; a second channel is formed between the first partition plate and the second partition plate, and a second gas-liquid contact inner member 11 is arranged in the second channel; a third channel is formed between the second clapboard and the tower wall, and a third gas-liquid contact internal part 12 is arranged in the third channel; wherein the first partition enables the first channel to have a single overhead, and the first partition and the second partition enable the second channel and the third channel to have a common overhead; the first channel and the second channel are provided with a common tower kettle by the first clapboard, and the third channel is provided with an independent tower kettle by the second clapboard; a first channel and a second channel common tower kettle are connected with a first reboiler 2 through a first circulating pump 4, a third channel tower kettle is connected with a second reboiler 3 through a second circulating pump 5, the top of the first channel tower is connected with a first condenser 6, and the top of the second channel and the third channel common tower is connected with a second condenser 7.
In the technical scheme, the proportion range of the sectional area of each channel in the sectional area of the rectifying tower is independently selected to be 10-90%.
In the above technical scheme, the first to fourth channel internal gas-liquid contact members are selected from trays or packing.
In the technical scheme, the first channel gas-liquid contact internal member to the fourth channel gas-liquid contact internal member are selected from tower plates, and the number of the tower plates is 15-35.
In the technical scheme, the first channel gas-liquid contact internal part to the fourth channel gas-liquid contact internal part are selected from fillers, and the theoretical plate number of the fillers is 15-35.
In order to solve the second technical problem, the technical scheme adopted by the invention is not as follows: an organic solvent purification processing method using any one of the above technical solutions to solve the technical problems, comprising the steps of:
1) introducing the organic solvent waste liquid (A) into a first channel of a rectifying tower, obtaining a qualified light component (B) at the top of the first channel tower, and obtaining a tower bottom liquid containing the organic solvent with the concentration not lower than 80% in percentage by mass at the tower bottom of the first channel;
2) evaporating the tower bottom liquid obtained in the step 1) through a first reboiler, evaporating partial steam to the top of the tower through a first channel, condensing the steam through a first condenser, extracting one part of the steam serving as qualified light components (B), and refluxing one part of the steam (E); another part of the steam reaches the top of the common tower of the second channel and the third channel through the second channel, is condensed through a second condenser, and is redistributed to the second channel and the third channel in a reflux mode (F, G); the other part is taken out as an intermediate component (C), and the taken-out intermediate component can be independently treated and can also be mixed with the organic solvent waste liquid A for recycling;
3) and concentrating the redistributed organic solvent solution through a third channel, and obtaining an organic solvent solution (D) with the organic solvent concentration of not less than 99.5 percent in a third channel tower kettle according to the mass percent, and extracting the organic solvent solution (D) as a final organic solvent product.
In the technical scheme, the proportion of the steam evaporated to the first channel and the second channel in the step 2) is in direct proportion to the cross section area of the channels, and the proportion value is 1/10-9/10.
In the above technical solution, the proportion of the organic solvent solution condensed in step 2) redistributed to the second channel and the third channel in a reflux manner is proportional to the cross-sectional area of the channels, and the proportion is 1/10-9/10.
In the above technical scheme, the evaporation conditions of the distillation column in step 2) shared by the first channel and the second channel of the distillation column are as follows: the operation pressure is 1KPa to 100KPa, and the operation temperature is 30 ℃ to 160 ℃.
In the above technical scheme, the evaporation conditions of the third channel tower kettle of the rectifying tower in the step 3) are as follows: the operation pressure is 1KPa to 100KPa, and the operation temperature is 30 ℃ to 160 ℃.
In the technical scheme, the reflux ratio in the step 2) is independently selected from 0.1-10.
In the technical scheme, the organic solvent is dimethyl sulfoxide, wherein the tower top temperature of the first channel is 10-50 ℃, and the tower top temperature of the second channel and the third channel is 20-100 ℃.
By adopting the technical scheme of the invention, the traditional three-tower process flow is replaced by one tower, the process flow is greatly simplified, and the reboiler and the condenser are saved, so that the energy consumption is greatly reduced, and a better technical effect is obtained.
Drawings
FIG. 1 is a process flow of the present invention.
In the figure, 1 is a three-channel rectification column, 2 is a first reboiler, 3 is a second reboiler, 4 is a first circulation pump, 5 is a second circulation pump, 6 is a first condenser, 7 is a second condenser, 8 is a first partition plate, 9 is a second partition plate, 10 is a first gas-liquid contact internal member, 11 is a second gas-liquid contact internal member, and 12 is a third gas-liquid contact internal member.
A is organic solvent waste liquid, B is qualified light component, C is intermediate component, D is synthetic organic solvent product, E is first channel backflow, F is second channel backflow, and G is third channel backflow.
FIG. 2 shows a rectifying column used in comparative example 1, in which a partition is provided in the middle.
FIG. 3 shows a rectifying column used in comparative example 2 with two partitions in the middle.
FIG. 4 shows a rectifying column used in comparative example 3 with three partitions in the middle.
The following description will further describe the specific embodiments of the present invention with reference to the drawings.
Detailed Description
The following is a detailed description of embodiments of the invention: the present example is carried out on the premise of the technical solution of the present invention, and detailed embodiments and processes are given, but the scope of the present invention is not limited to the following examples, and the process parameters of specific conditions not noted in the following examples are generally in accordance with conventional conditions.
[ example 1 ]
According to the apparatus of FIG. 1, the gas-liquid inside the column contacts the trays of the internals, the number of trays is 30, and the specific operating parameters of the column are: the pressure of the tower is controlled at 1KPa, wherein the temperature of the tower kettle shared by the first channel and the second channel is controlled at 75 ℃, the temperature of the tower kettle of the third channel is controlled at 92 ℃, the temperature of the tower top of the first channel is controlled at 25 ℃, the temperature of the tower top shared by the second channel and the third channel is controlled at 39 ℃, the reflux ratio of the first channel is 4, and the reflux ratio of the second channel and the third channel is 9.
The weight percent compositions, process parameters and dimethyl sulfoxide yields of the raw materials and components of the various streams used in this example are shown in tables 1.1 and 1.2
TABLE 1.1
TABLE 1.2
[ example 2 ]
According to the apparatus of FIG. 1, the gas-liquid inside the column contacts the trays of the internals, the number of trays is 25, and the specific operating parameters of the column are: the pressure of the tower is controlled at 6KPa, wherein the temperature of the tower kettle shared by the first channel and the second channel is controlled at 80 ℃, the temperature of the tower kettle of the third channel is controlled at 107 ℃, the temperature of the tower top of the first channel is controlled at 28 ℃, the temperature of the tower top shared by the second channel and the third channel is controlled at 43 ℃, the reflux ratio of the first channel is 5, and the reflux ratio of the condensation shared by the second channel and the third channel is 7.
The weight percent compositions, process parameters and dimethyl sulfoxide yields of the raw materials and components of the various streams used in this example are shown in tables 2.1 and 2.2
TABLE 2.1
TABLE 2.2
[ example 3 ]
According to the apparatus of FIG. 1, the gas-liquid inside the column contacts the trays of the internals, the number of trays is 25, and the specific operating parameters of the column are: the pressure of the tower is controlled at 9KPa, wherein the temperature of the tower kettle shared by the first channel and the second channel is controlled at 85 ℃, the temperature of the tower kettle shared by the third channel and the fourth channel is controlled at 117 ℃, the temperature of the tower top of the first channel is controlled at 31 ℃, the temperature of the tower top shared by the second channel and the third channel is controlled at 20 ℃, the reflux ratio of the first channel is 2, and the reflux ratio of the condensation shared by the second channel and the third channel is 5.
The weight percent compositions, process parameters and dimethyl sulfoxide yields of the feed and stream components used in this example are shown in tables 3.1 and 3.2
TABLE 3.1
TABLE 3.2
[ example 4 ]
According to the apparatus of FIG. 1, the gas-liquid inside the column contacts the trays of the internals, the number of trays is 25, and the specific operating parameters of the column are: the pressure of the tower is controlled at 22KPa, wherein the temperature of the tower kettle shared by the first channel and the second channel is controlled at 124 ℃, the temperature of the tower kettle of the third channel is controlled at 142 ℃, the temperature of the tower top of the first channel is controlled at 48 ℃, the temperature of the tower top shared by the second channel and the third channel is controlled at 64 ℃, the reflux ratio of the first channel is 5, and the reflux ratio of the fourth channel is 3.
The weight percent compositions, process parameters and dimethyl sulfoxide yields of the feed and stream components used in this example are shown in tables 4.1 and 4.2
TABLE 4.1
TABLE 4.2
Comparative example 1
The comparative example is the rectifying tower of fig. 2, a baffle is arranged in the tower, the baffle is positioned in the middle, gas and liquid in the tower contact internal member tower plates, the number of the tower plates is 30, and the specific operating parameters of the tower are as follows: the pressure of the tower is controlled at 1KPa, wherein the temperature of the kettle of the tower is controlled at 92 ℃, the temperature of the top of the tower is controlled at 63 ℃, and the reflux ratio is 4.
The weight percent composition, light transmittance, process parameters, and dimethyl sulfoxide yield of the raw materials and components of each stream used in this example are shown in table 5.
TABLE 5
Comparative example 2
The comparative example is the rectification column of fig. 3, with two baffles in the middle, gas-liquid contact internals trays in the column, the number of trays being 30, the specific operating parameters of the column being: the pressure of the tower is controlled at 1KPa, wherein the temperature of the kettle of the tower is controlled at 92 ℃, the temperature of the top of the tower is controlled at 63 ℃, and the reflux ratio is 4.
The weight percent composition, light transmittance, process parameters, and dimethyl sulfoxide yield of the raw materials and components of each stream used in this example are shown in table 6.
TABLE 6
Comparative example 3
The comparative example is the rectification column of fig. 4, with three baffles in the middle, the gas and liquid in the column contacting the trays of the internals, the number of trays being 30, the specific operating parameters of the column being: the pressure of the tower is controlled at 1KPa, wherein the temperature of the kettle of the tower is controlled at 92 ℃, the temperature of the top of the tower is controlled at 63 ℃, and the reflux ratio is 4.
The weight percent composition, light transmittance, process parameters, and dimethyl sulfoxide yield of the raw materials and components of each stream used in this example are shown in table 7.
TABLE 7
It can be seen from the above comparative example that the position of the partition board has a great influence on the purity of the product of the rectifying tower, and the suspended partition board in the comparative example may cause the mixing of the pure components at the top or bottom of the tower, so that the product is difficult to achieve a high purity (not less than 99.5%).
The analytical results of dimethyl sulfoxide used in the polymerization of carbon fibers and dimethyl sulfoxide obtained by the process were compared, as shown in Table 8
TABLE 8
| Item | Index of commercial DMSO raw Material | Example 1 | Example 2 | Example 3 | Example 4 |
| Water (%) | 0.09 | 0.08 | 0.06 | 0.04 | 0.03 |
| DMSO(％) | 99.88 | 99.92 | 99.94 | 99.96 | 99.97 |
| Polymer (%) | Not detected out | Not detected out | Not detected out | Not detected out | Not detected out |
| Acrylonitrile (%) | Not detected out | Not detected out | Not detected out | Not detected out | Not detected out |
| Na ion (μ g/g) | 0.09 | 0.05 | 0.06 | 0.06 | 0.07 |
| K ion (μ g/g) | 0.03 | 0.01 | 0.02 | 0.02 | 0.02 |
| Ca ion (μ g/g) | 0.21 | 0.02 | 0.02 | 0.04 | 0.03 |
| Mg ion (μ g/g) | 0.06 | 0.01 | 0.01 | 0.01 | 0.01 |
| Fe ion (μ g/g) | 0.06 | 0.02 | 0.04 | 0.03 | 0.02 |
In summary, as can be seen from the data in table 8, the device and the method for purifying an organic solvent, particularly used in a process of purifying dimethyl sulfoxide, can effectively purify and recover dimethyl sulfoxide waste liquid (including but not limited to dimethyl sulfoxide solvent for polymerization, kettle washing liquid for polymerization kettle, and sulfoxide waste liquid for coagulation bath) generated in a carbon fiber production process, and each index of the purified dimethyl sulfoxide is equivalent to or superior to that of commercial dimethyl sulfoxide. The invention effectively recovers the dimethyl sulfoxide, reduces the production cost, and simultaneously, the recovered water can be recycled, thereby reducing the pollution to the environment.
Claims (13)
1. An organic solvent purification device comprises a rectifying tower (1), a first reboiler (2), a second reboiler (3), a first condenser (6) and a second condenser (7); the device is characterized in that at least a first clapboard (8) and a second clapboard (9) are arranged in the rectifying tower (1), a first channel is formed between the first clapboard and the tower wall, and a first gas-liquid contact internal part (10) is arranged in the first channel; a second channel is formed between the first clapboard and the second clapboard, and a second gas-liquid contact internal part (11) is arranged in the second channel; a third channel is formed between the second clapboard and the tower wall, and a third gas-liquid contact internal part (12) is arranged in the third channel; wherein the first partition enables the first channel to have a single overhead, and the first partition and the second partition enable the second channel and the third channel to have a common overhead; the first channel and the second channel are provided with a common tower kettle by the first clapboard, and the third channel is provided with an independent tower kettle by the second clapboard; a first channel and a second channel are connected with a first reboiler (2) through a first circulating pump (4), a third channel is connected with a second reboiler (3) through a second circulating pump (5), a first condenser (6) is connected to the top of the first channel, and a second condenser (7) is connected to the top of the second channel and the third channel.
2. The organic solvent recovery processing device according to claim 1, wherein the ratio of the sectional area of each passage to the sectional area of the rectifying tower is independently selected to be 10% to 90%.
3. The organic solvent recovery processing apparatus according to claim 1, wherein the first-fourth channel internal gas-liquid contact member is selected from a tray or a packing.
4. The apparatus for recovering and treating an organic solvent according to claim 3, wherein the first channel vapor-liquid contacting internals to the fourth channel vapor-liquid contacting internals are selected from trays having a number of 15 to 35.
5. The apparatus for recovering and treating an organic solvent according to claim 3, wherein the first to fourth channel internal vapor-liquid contact members are selected from packing materials having a theoretical plate number of 15 to 35.
6. An organic solvent purification method for purifying an organic solvent by using the organic solvent purification device comprises the following steps:
1) introducing the organic solvent waste liquid (A) into a first channel of a rectifying tower, obtaining a qualified light component (B) at the top of the first channel tower, and obtaining a tower bottom liquid containing the organic solvent with the concentration not lower than 80% in percentage by mass at the tower bottom of the first channel;
2) evaporating the tower bottom liquid obtained in the step 1) through a first reboiler, evaporating partial steam to the top of the tower through a first channel, condensing the steam through a first condenser, extracting one part of the steam serving as qualified light components (B), and refluxing one part of the steam (E); another part of the steam reaches the top of the common tower of the second channel and the third channel through the second channel, is condensed through a second condenser, and is redistributed to the second channel and the third channel in a reflux mode (F, G); the other part is taken out as an intermediate component (C), and the taken-out intermediate component is optionally independently treated or mixed with the organic solvent waste liquid A for recycling;
3) the redistributed organic solvent solution passes through a third channel, and an organic solvent solution (D) with the organic solvent concentration not lower than 99.5 percent is obtained in a third channel tower kettle according to the mass percentage and is taken out as a final organic solvent product.
7. The organic solvent recovery processing method according to claim 6, wherein the ratio of the steam evaporated to the first channel and the second channel in the step 2) is proportional to the channel cross-sectional area, and the ratio is between 1/10 and 9/10.
8. The organic solvent recovery processing method according to claim 6, wherein the distribution ratio of the organic solvent solution condensed in step 2) to the second channel and the third channel in a reflux manner is proportional to the channel cross-sectional area, and the value of the ratio is 1/10-9/10.
9. The organic solvent recovery processing method according to claim 6, wherein the common bottom evaporation conditions of the first channel and the second channel of the rectifying tower in the step 2) are as follows: the operation pressure is 1KPa to 100KPa, and the operation temperature is 30 ℃ to 160 ℃.
10. The organic solvent recovery processing method according to claim 6, wherein the evaporation conditions of the third channel still of the rectifying tower in the step 3) are as follows: the operation pressure is 1KPa to 100KPa, and the operation temperature is 30 ℃ to 160 ℃.
11. The method according to claim 6, wherein the reflux ratio in the step 2) is independently selected from 0.1 to 10.
12. The method for recovering and treating an organic solvent according to any one of claims 6 to 11, wherein the organic solvent is dimethyl sulfoxide.
13. The organic solvent recovery processing method according to claim 12, wherein the first channel overhead temperature is 10 to 50 ℃, and the second channel and the third channel overhead temperature is 20 to 100 ℃.
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