CN112221181A - Organic solvent recovery processing device and processing method - Google Patents

Organic solvent recovery processing device and processing method Download PDF

Info

Publication number
CN112221181A
CN112221181A CN201910638088.2A CN201910638088A CN112221181A CN 112221181 A CN112221181 A CN 112221181A CN 201910638088 A CN201910638088 A CN 201910638088A CN 112221181 A CN112221181 A CN 112221181A
Authority
CN
China
Prior art keywords
channel
organic solvent
tower
liquid contact
clapboard
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910638088.2A
Other languages
Chinese (zh)
Inventor
王清立
顾军民
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
Original Assignee
China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Petroleum and Chemical Corp, Sinopec Shanghai Research Institute of Petrochemical Technology filed Critical China Petroleum and Chemical Corp
Priority to CN201910638088.2A priority Critical patent/CN112221181A/en
Publication of CN112221181A publication Critical patent/CN112221181A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/141Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B01D3/324Tray constructions
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C315/00Preparation of sulfones; Preparation of sulfoxides
    • C07C315/06Separation; Purification; Stabilisation; Use of additives

Abstract

The invention relates to an organic solvent recovery processing device and a processing method, which mainly solve the problems of longer process flow, higher equipment investment and energy consumption in the prior art, and adopts the organic solvent recovery processing device which comprises a rectifying tower, a first reboiler, a second reboiler, a first condenser, a second condenser and a third condenser; the method is characterized in that at least a first clapboard, a second clapboard and a third clapboard are arranged in the rectifying tower, a first channel is formed between the first clapboard and the tower wall, and a first gas-liquid contact internal part 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 internal part is arranged in the second channel; a third channel is formed between the second partition plate and the third partition plate, and a third gas-liquid contact internal part is arranged in the third channel; the fourth channel is formed between the fourth clapboard and the tower wall, and the fourth gas-liquid contact internal part is arranged in the fourth channel, so that the problem is better solved, and the organic solvent recovery tower can be used in the industrial application of organic solvent recovery treatment.

Description

Organic solvent recovery processing device and processing method
Technical Field
The invention relates to an organic solvent recovery processing device and a processing method, in particular to a dimethyl sulfoxide recovery processing method and a dimethyl sulfoxide recovery processing device.
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. The process has the advantages of long flow, complex operation and high energy consumption, and the dimethyl sulfoxide obtained by the process has purity and metal ion content reaching the dimethyl sulfoxide recycling standard, but light transmittance is not considered, so that the dimethyl sulfoxide suitable for carbon fiber polymerization production has high requirements on reducing impurities and metal ions and strict requirements on light transmittance.
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 and refining 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 that: the process flow is longer, the energy consumption is higher, and the transmittance of the obtained product is not described.
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 recovery processing 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 recovery processing device comprises a rectifying tower 1, a first reboiler 2, a second reboiler 3, a first condenser 6, a second condenser 7 and a third condenser 8; at least a first clapboard 9, a second clapboard 10 and a third clapboard 11 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 16 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 17 is arranged in the second channel; a third channel is formed between the second partition plate and the third partition plate, and a third gas-liquid contact internal member 18 is arranged in the third channel; a fourth channel is formed between the fourth clapboard and the tower wall, and a fourth gas-liquid contact internal piece 19 is arranged in the fourth channel; wherein the first partition enables the first channel to have a single overhead, the fourth partition enables the fourth channel to have a single overhead, and the first partition and the fourth partition enable the second channel and the third channel to have a common overhead; the first channel, the second channel, the third channel and the fourth channel are respectively provided with mutually independent common tower kettles by the second partition plate; a first channel and second channel common tower kettle is connected with a first reboiler 2 through a first circulating pump 4, a third channel and fourth channel common tower kettle is connected with a second reboiler 3 through a second circulating pump 5, the top of the first channel is connected with a first condenser 6, the top of the second channel and third channel common tower is connected with a second condenser 7, and the top of the fourth channel common tower is connected with a third condenser 8.
In the technical scheme, the proportion range of the sectional area of each channel in the sectional area of the rectifying tower is independently and preferably 10-90%.
In the above technical solution, the first internal gas-liquid contact member, the second internal gas-liquid contact member, the third internal gas-liquid contact member, and the fourth internal gas-liquid contact member are independently preferably selected from a tray or a packing.
In the above technical scheme, the first internal gas-liquid contact member, the second internal gas-liquid contact member, the third internal gas-liquid contact member and the fourth internal gas-liquid contact member are preferably selected from trays, and the number of the trays is preferably 15 to 35.
In the above technical solution, the first internal gas-liquid contact member, the second internal gas-liquid contact member, the third internal gas-liquid contact member, and the fourth internal gas-liquid contact member are independently selected from packing, and the number of theoretical plates of the packing is preferably 15 to 35.
In order to solve the second problem, the invention is realized by the following technical scheme: an organic solvent recovery processing method using any one of the above-described 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 tower bottom liquid containing the organic solvent with the concentration not lower than 80% at the tower bottom of the first channel tower according to the mass percentage;
2) evaporating the tower bottom liquid obtained in the step 1) through a first reboiler, evaporating part of steam to the top of the tower through a first channel, condensing the steam through a first condenser, extracting one part of steam serving as qualified light component (B), and refluxing one part of steam; the other 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;
3) the redistributed organic solvent solution passes through a third channel, and an organic solvent solution with the organic solvent concentration not lower than 99.5 percent is obtained in a tower kettle shared by the third channel and a fourth channel according to the mass percentage;
4) evaporating the organic solvent solution obtained in the step 3) by a second reboiler, allowing part of the organic solvent solution to pass through a third channel, allowing the other part of the organic solvent solution to pass through a fourth channel, condensing the organic solvent solution by a third condenser, allowing part of the organic solvent solution to be used as reflux, and collecting part of the organic solvent solution serving as a final organic solvent product (C).
In the technical scheme, the proportion of the steam evaporated to the first channel and the second channel in the step 2) is preferably 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 distribution ratio of the organic solvent solution condensed in step 2) redistributed to the second channel and the third channel in a reflux manner is preferably proportional to the channel cross-sectional area, and the ratio is 1/10-9/10.
In the technical scheme, the proportion of the steam evaporated to the third channel and the fourth channel in the step 3) is preferably 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, in the step 2), the evaporation conditions of the distillation column shared by the first channel and the second channel are preferably: the operation pressure is 1KPa to 100KPa, and the operation temperature is 30 ℃ to 160 ℃.
In the above technical solution, in the step 3), the evaporation conditions of the distillation column shared by the third channel and the fourth channel are preferably: the operation pressure is 1KPa to 100KPa, and the operation temperature is 30 ℃ to 160 ℃.
In the above technical scheme, the reflux ratio in the step 1) and the step 4) is independently preferably selected from 0.1-10.
In the above technical solution, the organic solvent may be any one of dimethylformamide, dimethylacetamide and dimethylsulfoxide; further preferably dimethyl sulfoxide, wherein the tower top temperature of the first channel is preferably 10-50 ℃, the tower top temperature of the second channel and the third channel is preferably 20-90 ℃, and the tower top temperature of the fourth channel is preferably 50-100 ℃.
By adopting the technical scheme of the invention, through the arranged organic solvent recovery and treatment device, the traditional three-tower process flow is replaced by one tower, the process flow is greatly simplified, and a reboiler and a 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 four-channel rectifying 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 third condenser, 9 is a first partition, 10 is a second partition, 11 is a third partition, 12 is a first gas-liquid contact internal, 13 is a second gas-liquid contact internal, 14 is a third gas-liquid contact internal, and 15 is a fourth gas-liquid contact internal.
A is organic solvent waste liquid, B is qualified light component, C is organic solvent product, D is residual liquid, E is first channel backflow, F is second channel backflow, G is third channel backflow, and H is fourth 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 first tower kettle is controlled at 75 ℃, the temperature of the second tower kettle is controlled at 92 ℃, the temperature of the top of the first channel is controlled at 25 ℃, the temperature of the top of the second channel and the third channel which share the same tower is controlled at 39 ℃, the temperature of the top of the fourth channel is controlled at 63 ℃, the reflux ratio of the first channel is 4, and the reflux ratio of the fourth channel is 0.3.
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 tables 1.1 and 1.2.
TABLE 1.1
Figure RE-GDA0002369358450000061
TABLE 1.2
Figure RE-GDA0002369358450000062
[ 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 first tower kettle is controlled at 80 ℃, the temperature of the second tower kettle is controlled at 107 ℃, the temperature of the top of the first channel is controlled at 28 ℃, the common top of the second channel and the third channel is controlled at 43 ℃, the top of the fourth channel is controlled at 68 ℃, the reflux ratio of the first channel is 5, and the reflux ratio of the fourth channel is 1.
The weight percent composition, transmittance, process parameters and dimethyl sulfoxide yield of the raw materials and components of each stream used in this example are shown in tables 2.1 and 2.2
TABLE 2.1
Figure RE-GDA0002369358450000071
TABLE 2.2
Figure RE-GDA0002369358450000072
[ 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 first tower kettle is controlled at 85 ℃, the temperature of the second tower kettle is controlled at 117 ℃, the temperature of the top of the first channel is controlled at 31 ℃, the common top of the second channel and the third channel is controlled at 20 ℃, the top of the fourth channel is controlled at 75 ℃, the reflux ratio of the first channel is 2, and the reflux ratio of the fourth channel is 0.5.
The weight percent composition, transmittance, process parameters, and dimethyl sulfoxide yield of the raw materials and components of each stream used in this example are shown in tables 3.1 and 3.2
TABLE 3.1
Figure RE-GDA0002369358450000073
TABLE 3.2
Figure RE-GDA0002369358450000081
[ 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 first tower kettle is controlled at 124 ℃, the temperature of the second tower kettle is controlled at 142 ℃, the temperature of the first channel tower top is controlled at 48 ℃, the temperature of the second channel tower top and the third channel tower top are controlled at 64 ℃, the temperature of the fourth channel tower top is controlled at 95 ℃, the reflux ratio of the first channel is 5, and the reflux ratio of the fourth channel is 1.5.
The weight percent composition, transmittance, process parameters and dimethylsulfoxide yields of the raw materials and the individual stream components used in this example are shown in tables 4.1 and 4.2
TABLE 4.1
Figure RE-GDA0002369358450000082
TABLE 4.2
Figure RE-GDA0002369358450000083
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
Figure RE-GDA0002369358450000091
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
Figure RE-GDA0002369358450000092
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
Figure RE-GDA0002369358450000101
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 0.05 0.04 0.04 0.04
DMSO(%) 99.88 99.95 99.96 99.96 99.96
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 0.12 0.05 0.09 0.11
K ion (μ g/g) 0.03 0.02 0.01 0.01 0.04
Ca ion (μ g/g) 0.21 0.07 0.03 0.09 0.03
Mg ion (μ g/g) 0.06 0.01 0.01 0.01 0.02
Fe ion (μ g/g) 0.06 0.03 0.01 0.02 0.01
Transmittance at 400nm (%) 96 99.8 99.8 99.7 99.6
In summary, as can be seen from the data in table 8, the apparatus and method for recovering an organic solvent according to the present invention, particularly when used in a process of recovering dimethyl sulfoxide, can effectively 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 recovered 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 (14)

1. An organic solvent recovery processing device comprises a rectifying tower (1), a first reboiler (2), a second reboiler (3), a first condenser (6), a second condenser (7) and a third condenser (8); the device is characterized in that at least a first clapboard (9), a second clapboard (10) and a third clapboard (11) 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 (12) 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 (13) is arranged in the second channel; a third channel is formed between the second clapboard and the third clapboard, and a third gas-liquid contact internal part (14) is arranged in the third channel; a fourth channel is formed between the fourth clapboard and the tower wall, and a fourth gas-liquid contact internal part (15) is arranged in the fourth channel; wherein the first partition enables the first channel to have a single overhead, the fourth partition enables the fourth channel to have a single overhead, and the first partition and the fourth partition enable the second channel and the third channel to have a common overhead; the first channel, the second channel, the third channel and the fourth channel are respectively provided with mutually independent common tower kettles by the second partition plate; 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 and a fourth channel common tower kettle are 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, a second condenser (7) is connected to the top of the second channel and the third channel common tower, and a third condenser (8) is connected to the top of the fourth channel common tower.
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 apparatus according to claim 1, wherein the first internal gas-liquid contact member, the second internal gas-liquid contact member, the third internal gas-liquid contact member, and the fourth internal gas-liquid contact member are independently selected from trays and packing.
4. The apparatus according to claim 3, wherein the first internal gas-liquid contact member, the second internal gas-liquid contact member, the third internal gas-liquid contact member and the fourth internal gas-liquid contact member are independently selected from trays, and the number of the trays is 15 to 35.
5. The apparatus according to claim 3, wherein the first internal gas-liquid contact member, the second internal gas-liquid contact member, the third internal gas-liquid contact member and the fourth internal gas-liquid contact member are independently selected from packing materials, and the number of theoretical plates of the packing materials is 15 to 35.
6. An organic solvent recovery processing method using the organic solvent recovery processing apparatus according to any one of claims 1 to 5, 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 portion of the vapor passes through the second pass to the common overhead of the second pass and the third pass, is condensed by a second condenser, and is redistributed to the second pass and the third pass as reflux (F, G);
3) the redistributed organic solvent solution passes through a third channel, and an organic solvent solution with the organic solvent concentration not lower than 99.5 percent is obtained in a tower kettle shared by the third channel and a fourth channel according to the mass percentage;
4) evaporating the organic solvent solution obtained in the step 3) by a second reboiler, allowing part of the organic solvent solution to pass through a third channel, allowing the other part of the organic solvent solution to pass through a fourth channel, condensing the organic solvent solution by a third condenser, taking part of the organic solvent solution as reflux (H), and taking part of the organic solvent solution as a final organic solvent product (C) for extraction.
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 ratio of the steam evaporated to the third channel and the fourth channel in the step 3) is proportional to the channel cross-sectional area, and the ratio is between 1/10 and 9/10.
10. 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 ℃.
11. The organic solvent recovery processing method according to claim 6, wherein the evaporation conditions of the shared bottom of the third channel and the fourth channel 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 ℃.
12. The method for recovering and treating an organic solvent according to claim 6, wherein the reflux ratio in the step 1) and the step 4) is independently selected from 0.1 to 10.
13. The method for recovering and treating an organic solvent according to any one of claims 6 to 12, wherein the organic solvent is any one of dimethylformamide, dimethylacetamide and dimethylsulfoxide; further preferred is dimethyl sulfoxide.
14. The organic solvent recovery processing method according to claim 13, wherein the first channel overhead temperature is 10 to 50 ℃, the second channel and third channel overhead temperature is 20 to 90 ℃, and the fourth channel overhead temperature is 50 to 100 ℃.
CN201910638088.2A 2019-07-15 2019-07-15 Organic solvent recovery processing device and processing method Pending CN112221181A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910638088.2A CN112221181A (en) 2019-07-15 2019-07-15 Organic solvent recovery processing device and processing method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910638088.2A CN112221181A (en) 2019-07-15 2019-07-15 Organic solvent recovery processing device and processing method

Publications (1)

Publication Number Publication Date
CN112221181A true CN112221181A (en) 2021-01-15

Family

ID=74111171

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910638088.2A Pending CN112221181A (en) 2019-07-15 2019-07-15 Organic solvent recovery processing device and processing method

Country Status (1)

Country Link
CN (1) CN112221181A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112225680A (en) * 2019-07-15 2021-01-15 中国石油化工股份有限公司 Organic solvent purification method and device

Citations (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001334101A (en) * 2000-05-29 2001-12-04 Kyowa Yuka Kk Distillation apparatus and distillation method using the same
JP2001353401A (en) * 2000-06-14 2001-12-25 Kyowa Yuka Kk Distillation apparatus and distillation method using the same
JP2003220301A (en) * 2002-01-30 2003-08-05 Jgc Corp Distillation purifying method
EP1371633A1 (en) * 2002-06-14 2003-12-17 Bayer Ag Process for the purification of mixtures of toluenediisocyanate incorporating a dividing-wall distillation column
EP1681094A2 (en) * 2005-01-17 2006-07-19 Basf Aktiengesellschaft Reactor with two or more separate reaction chambers
CN1809520A (en) * 2003-05-20 2006-07-26 巴斯福股份公司 Method for obtaining crude 1,3-butadiene from a C4
US20070043217A1 (en) * 2003-10-17 2007-02-22 Basf Aklengesellschaft Method for the distillative separation of mixtures containing ethyleneamines
CN101367720A (en) * 2008-09-18 2009-02-18 中国石油大学(华东) Acrylic purification process and apparatus of bulkhead azeotropy rectification column
CN101927097A (en) * 2009-06-22 2010-12-29 巴斯夫欧洲公司 By in having the tower of one or more continuous partition walls, distilling the method for separating one or more incoming mixtures
US20110168542A1 (en) * 2008-09-17 2011-07-14 Basf Se Devices and method for continuous distillative separation of a mixture containing one or more alkanolamine(s)
US20130267751A1 (en) * 2010-10-11 2013-10-10 Stefano Favilli Process and equipment for separating 1,2,4 trimethylbenzene (pseudocumene) from a mixture containing aromatic hydrocarbons
CN103664481A (en) * 2013-11-11 2014-03-26 天津科林泰克科技有限公司 Method for refining petrobenzene and thiophene by adopting double-partition-wall extraction rectifying tower
CN105749575A (en) * 2014-12-17 2016-07-13 新特能源股份有限公司 Divided wall distillation column for recovery of tail gas absorption liquid and condensate liquid in polysilicon production, method and processing system
CN105771295A (en) * 2016-05-19 2016-07-20 河北工业大学 Separation plate tower capable of controlling gas-phase distribution ratio and used for separating four-component mixture
US20160263492A1 (en) * 2013-10-23 2016-09-15 China Petroleum & Chemical Corporation Divided-wall column
CN109320431A (en) * 2018-10-24 2019-02-12 福建师范大学福清分校 A method of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether in recycling paint stripper waste liquid
CN109320417A (en) * 2018-11-29 2019-02-12 武汉有机实业有限公司 Utilize the device and method of partition tower purification Ergol
US20190091600A1 (en) * 2017-09-28 2019-03-28 Exxonmobil Research And Engineering Company Dual-dividing wall column with multiple products
CN208898768U (en) * 2018-09-18 2019-05-24 福建师范大学福清分校 The equipment of mixed acid waste water during a kind of extraction-partition wall rectification process Carboxylic Acid Fibre is plain
CN110002960A (en) * 2019-05-05 2019-07-12 北京化工大学 A kind of device and method of separation ABE fermentation infiltration evaporation liquid

Patent Citations (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001334101A (en) * 2000-05-29 2001-12-04 Kyowa Yuka Kk Distillation apparatus and distillation method using the same
JP2001353401A (en) * 2000-06-14 2001-12-25 Kyowa Yuka Kk Distillation apparatus and distillation method using the same
JP2003220301A (en) * 2002-01-30 2003-08-05 Jgc Corp Distillation purifying method
EP1371633A1 (en) * 2002-06-14 2003-12-17 Bayer Ag Process for the purification of mixtures of toluenediisocyanate incorporating a dividing-wall distillation column
US20030230476A1 (en) * 2002-06-14 2003-12-18 Bill Brady Process for the purification of mixtures of toluenediisocyanate incorporating a dividing-wall distillation column
CN1809520A (en) * 2003-05-20 2006-07-26 巴斯福股份公司 Method for obtaining crude 1,3-butadiene from a C4
US20070043217A1 (en) * 2003-10-17 2007-02-22 Basf Aklengesellschaft Method for the distillative separation of mixtures containing ethyleneamines
EP1681094A2 (en) * 2005-01-17 2006-07-19 Basf Aktiengesellschaft Reactor with two or more separate reaction chambers
US20110168542A1 (en) * 2008-09-17 2011-07-14 Basf Se Devices and method for continuous distillative separation of a mixture containing one or more alkanolamine(s)
CN101367720A (en) * 2008-09-18 2009-02-18 中国石油大学(华东) Acrylic purification process and apparatus of bulkhead azeotropy rectification column
CN101927097A (en) * 2009-06-22 2010-12-29 巴斯夫欧洲公司 By in having the tower of one or more continuous partition walls, distilling the method for separating one or more incoming mixtures
US20130267751A1 (en) * 2010-10-11 2013-10-10 Stefano Favilli Process and equipment for separating 1,2,4 trimethylbenzene (pseudocumene) from a mixture containing aromatic hydrocarbons
US20160263492A1 (en) * 2013-10-23 2016-09-15 China Petroleum & Chemical Corporation Divided-wall column
CN103664481A (en) * 2013-11-11 2014-03-26 天津科林泰克科技有限公司 Method for refining petrobenzene and thiophene by adopting double-partition-wall extraction rectifying tower
CN105749575A (en) * 2014-12-17 2016-07-13 新特能源股份有限公司 Divided wall distillation column for recovery of tail gas absorption liquid and condensate liquid in polysilicon production, method and processing system
CN105771295A (en) * 2016-05-19 2016-07-20 河北工业大学 Separation plate tower capable of controlling gas-phase distribution ratio and used for separating four-component mixture
US20190091600A1 (en) * 2017-09-28 2019-03-28 Exxonmobil Research And Engineering Company Dual-dividing wall column with multiple products
CN208898768U (en) * 2018-09-18 2019-05-24 福建师范大学福清分校 The equipment of mixed acid waste water during a kind of extraction-partition wall rectification process Carboxylic Acid Fibre is plain
CN109320431A (en) * 2018-10-24 2019-02-12 福建师范大学福清分校 A method of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether in recycling paint stripper waste liquid
CN109320417A (en) * 2018-11-29 2019-02-12 武汉有机实业有限公司 Utilize the device and method of partition tower purification Ergol
CN110002960A (en) * 2019-05-05 2019-07-12 北京化工大学 A kind of device and method of separation ABE fermentation infiltration evaporation liquid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王洪海;王宝正;李春利;姬鹏宇;: "垂直双隔板隔壁塔分离四组分的模拟优化和实验研究", 化工学报, no. 07 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112225680A (en) * 2019-07-15 2021-01-15 中国石油化工股份有限公司 Organic solvent purification method and device

Similar Documents

Publication Publication Date Title
CA2518809C (en) Ethanol distillation with distillers soluble solids recovery apparatus
RU2396242C2 (en) Method of methanol recuperation
CN105329961B (en) Low cost recovery DMF Waste Water Treatment
EP0055607B1 (en) Process for recovery of olefinic nitriles
CN108774163B (en) Method for recovering and purifying NMP (N-methyl pyrrolidone) in lithium battery production
CN108059597B (en) Method and device for producing ethyl acetate by integrating reactive distillation and pervaporation
CN107903148A (en) Top grade alcohol, alcohol fuel, electronic grade anhydrous alcohol production device and its production technology
CN101372381A (en) 3,3'-dichlorobenzidine hydrochloride waste water reclaiming method and apparatus thereof
CN112225680A (en) Organic solvent purification method and device
CN112624477A (en) Treatment device and treatment method for phenolic sodium salt decomposition wastewater
CN112142618B (en) Low-concentration dimethylformamide wastewater recovery system and method
US5711873A (en) Process for solvent recovery and apparatus suitable therefor
CN112221181A (en) Organic solvent recovery processing device and processing method
CN212051190U (en) Organic solvent purification device
CN111978233A (en) Device for improving purity of NMP crude product after methylamine removal
KR102466816B1 (en) Evaporation system comprising a series of evaporators for treating an ammoxidation process stream
CN107137949B (en) Extraction and rectification partition plate tower device and method for dehydrating low-concentration isopropanol solution
CN104844420A (en) Continuous treatment process and device of neopentyl glycol condensed washing mother liquor
CN212504671U (en) Device for improving purity of NMP crude product after methylamine removal
CN212504669U (en) Retrieve device of methylamine in follow NMP crude
CN107011141B (en) Process method for separating butyraldehyde, ethanol and water mixture
CN113426151A (en) Device and method for solvent DMSO rectification recovery process in carbon fiber production process
CN114057541B (en) Refining recovery method for dehydrating waste dichloromethane through supergravity coupling membrane
CN113979849B (en) Purification process for desulfurizing and dechlorinating 2-ethyl anthraquinone
US4714525A (en) Process for separating high purity water

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination