CN111617508B - GBL parallel flow multi-effect rectifying device - Google Patents
GBL parallel flow multi-effect rectifying device Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- C07D307/26—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D307/30—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings 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
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Abstract
GBL parallel flow multiple-effect rectifying device belongs to the technical field of chemical processes, and comprises a negative pressure dehydration tower and two rectifying towers, wherein the two rectifying towers are a rectifying high-pressure tower and a rectifying low-pressure tower respectively, the rectifying high-pressure tower and the rectifying low-pressure tower are connected in parallel, a tower top condenser of the rectifying high-pressure tower and a tower bottom reboiler of the rectifying low-pressure tower share a heat exchanger, steam is extracted from the tower top of the rectifying high-pressure tower and enters a tube side of the heat exchanger, liquid is extracted from the tower bottom of the rectifying low-pressure tower and is pumped into a shell side of the heat exchanger through a pump, and the heat exchanger is used as both a condenser of the rectifying high-pressure tower and a reboiler of the rectifying low-pressure tower, so that heat coupling is realized. The invention also discloses a corresponding GBL parallel flow multiple-effect rectification process, and the process has the advantages of good energy-saving effect, low equipment construction cost, low construction difficulty, low consumption of manpower and material resources and obvious effect.
Description
Technical Field
The invention belongs to the technical field of chemical processes, and particularly relates to a rectifying device and a method in a GBL production process.
Background
GBL (gamma-butyrolactone ) is an organic intermediate with wide application. The solvent is used as a high boiling point solvent and a proton type strong solvent and is used as a battery electrolyte to replace a strong corrosive acid liquid. Can also be used for preparing N-methyl pyrrolidone (NMP), butyric acid, amber paint remover and the like, and has wide application in the synthesis of fine chemicals such as medicines, spices and the like. The production route of GBL comprises processes such as a 1,4 Butanediol (BDO) dehydrogenation method, succinic anhydride hydro-dehydration and the like, and the BDO gas phase dehydrogenation method is widely adopted in China.
Dehydrogenation of 1, 4-butanediol
The BDO gas phase dehydrogenation method is to perform dehydrogenation reaction on BDO in a hydrogen atmosphere at the temperature of 230-240 ℃. The fixed bed tubular reactor filled with cylindrical particle copper catalyst is adopted, the single-pass conversion rate of 1, 4-butanediol is more than or equal to 97 percent, the selectivity of gamma-butyrolactone is more than or equal to 96 percent, and tetrahydrofuran is generated by side reaction with the selectivity less than 1 percent. And the crude GBL is subjected to continuous negative pressure rectification by a negative pressure dehydration tower and a rectification tower to prepare a pure GBL. The negative pressure dehydration tower removes light boiling and mainly comprises water (H)2O) and Tetrahydrofuran (THF). And the product with light boiling removed enters a rectifying tower to obtain GBL with the purity of 99.9 percent.
GBL purification is shown in FIG. 1, and crude product (C-GBL) after the reactor enters a negative pressure dehydration column T1, and light boiling (L-IMP, containing H2O and THF) is separated from the top of the column. The bottom of the tower is extracted and enters a rectifying tower T2, pure product P-GBL (the purity is more than or equal to 99.99%) is extracted from the top of the T2 tower, and reboiled (H-IMP) is extracted from the bottom of the tower. The recovery rate of GBL is more than 95%.
The process flow diagram of the above process is shown in fig. 2:
the main structural parameters of the column equipment used in the process are shown in table 1.
Table 1 GBL plant tower equipment main structure parameter table
The process flow and the equipment greatly improve the rectification recovery effect of GBL, but the energy consumption of the rectification tower is very high, so that the process and the equipment still need to be improved on the premise of not sacrificing the quality by people, and the requirements on environmental protection, energy conservation and emission reduction brought forward by people are more and more met.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a GBL parallel-flow multi-effect rectifying device.
The technical problem to be solved by the invention is realized by the following technical scheme:
GBL cocurrent flow multiple-effect rectification device, including negative pressure dehydration tower and two rectifying towers, two rectifying towers are rectification high pressure column and rectification low pressure column respectively, rectification high pressure column and rectification low pressure column parallel connection, be provided with the heat exchanger between rectification high pressure column and the rectification low pressure column, the overhead condenser of rectification high pressure column and the tower bottom reboiler of rectification low pressure column share a heat exchanger, wherein the top of the tower of rectification high pressure column is connected to the hot flow tube side of heat exchanger, the tower bottom of rectification low pressure column is connected to the cold flow shell side of heat exchanger, be provided with the backwash pump on the cold flow shell side.
In the invention, the theoretical stages of the rectification high-pressure tower are 42, the diameter of the tower is 650mm, the theoretical stages of the rectification low-pressure tower are 40, and the diameter of the tower is 1000 mm.
The GBL parallel flow multi-effect rectification process carried out by utilizing the equipment comprises the following steps:
(1) preheating the reacted GBL crude product by a preheater, feeding the preheated GBL crude product into the middle part of a negative pressure dehydration tower, removing light boiling in the negative pressure dehydration tower, distilling the light boiling out of the tower top of the negative pressure dehydration tower, feeding the light boiling into a THF (tetrahydrofuran) recovery process, and dividing heavy components into two parts after flowing out of the tower bottom of the negative pressure dehydration tower and respectively feeding the two parts into a rectifying high-pressure tower and a rectifying low-pressure tower;
(2) distilling the tower kettle extracted material entering the negative pressure dehydration tower of the rectification low pressure tower, extracting a pure product at the tower top, feeding the kettle liquid at the tower bottom into a cold flow shell pass of a heat exchanger for evaporation, feeding the gas-liquid mixture at the outlet into the tower kettle of the rectification low pressure tower, discharging the residual kettle liquid as reboiling, wherein the heat exchanger is used as a reboiler of the rectification low pressure tower at the moment, and the rectification low pressure tower obtains heat through the heat exchanger;
(3) the liquid enters a tower kettle of a negative pressure dehydration tower of the rectification high-pressure tower for extraction, the extraction liquid at the tower top enters a heat exchanger for condensation, the liquid leaves from a heat flow tube pass outlet of the heat exchanger, part of the solution is discharged as a pure product under the pushing of a reflux pump, part of the solution flows back to the tower top of the rectification high-pressure tower, the kettle liquid discharged at the tower bottom is discharged as reboiling, and the heat exchanger is used as a condenser of the rectification high-pressure tower at the moment and transfers heat to the tower kettle of the rectification low-pressure tower;
(4) the pure product coming from the top of the rectification high-pressure tower and subjected to heat exchange by the heat exchanger is converged with the pure product coming from the top of the rectification low-pressure tower and is discharged out of the equipment as a final product.
Further, the tower top pressure of the rectification high-pressure tower is 20kPa, and the tower top pressure of the rectification low-pressure tower is 3 kPa.
Further, the pressure drop of the rectification high-pressure tower is 5kPa, and the pressure drop of the rectification low-pressure tower is 3 kPa.
Further, the feeding position of the rectification high-pressure column is 39 stages from the top of the column, and the feeding position of the rectification low-pressure column is the bottom of the column.
Further, the reflux ratio of the rectification high-pressure column is 0.48.
Further, the heat exchange area of the heat exchanger is 9.675m2The inlet temperature of the heat flow tube pass of the heat exchanger is 147 ℃, and the inlet temperature of the cold flow shell pass of the heat exchanger is 102 ℃.
In the invention, a feed material flow enters a negative pressure dehydration tower for removing light boiling after being preheated, a tower kettle material flow is divided into two material flows which respectively enter a rectification high-pressure tower and a rectification low-pressure tower for parallel-flow double-effect distillation, and after condensation circulation and reboiling circulation, a product of the rectification high-pressure tower is combined with a tower top product of the rectification low-pressure tower along with the condensation circulation to be used as a final product of GBL rectification recovery.
Furthermore, the heat exchanger bears a condenser at the top of the rectification high-pressure tower and a reboiler at the bottom of the rectification low-pressure tower, and the load of the condenser of the rectification high-pressure tower is equal to that of the reboiler of the rectification low-pressure tower.
In the invention, two rectifying towers connected in parallel are adopted to share the rectifying work of GBL, and the tower top of the high-pressure rectifying tower is in cold-hot coupling with the tower kettle of the low-pressure tower, thus achieving good energy-saving effect; the heat exchanger connecting the condensation cycle and the reboiling cycle effectively exchanges heat, so that the condensation load and the reboiling load are reduced, under the same technical index, the load of the condenser is reduced by 58.75 percent on the original basis, the load of the reboiler is reduced by 63.48 percent, and the energy-saving effect is good; the heat exchange requirement on the heat exchanger is low; the size of the adopted double towers is far smaller than that of the existing rectifying tower, and the tower diameter is also far smaller than that of the existing rectifying tower, so that the construction cost of the equipment is greatly reduced, and the consumption of manpower and material resources is low.
Drawings
FIG. 1 is a flow diagram of a conventional GBL purification process;
FIG. 2 is a flow chart of the original GBL rectification recovery process;
FIG. 3 is a flow diagram of a GBL co-current multi-effect rectification process of the present invention;
FIG. 4 is a heat exchanger thermal analysis chart of the present invention;
FIG. 5 is a table of heat exchanger specifications according to the present invention;
FIG. 6 is a table of the hydraulics parameters of the GBL rectification higher pressure column T102NA tray of the present invention;
FIG. 7 is a table of the hydraulics parameters of the trays of GBL rectification lower pressure column T102NB of the present invention.
In the figure: negative pressure dehydration tower T1 (traditional technology), negative pressure dehydration tower T101 (former technology), negative pressure dehydration tower T101N, rectifying column T2 (traditional technology), rectifying column T102 (former technology), GBL rectification high pressure tower T102NA, GBL rectification low pressure tower T102NB, heat exchanger B9, preheater B15N.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
GBL parallel flow multiple-effect rectification device comprises a negative pressure dehydration tower T101N, a rectification high-pressure tower T102NA, a rectification low-pressure tower T102NB and a heat exchanger B9, wherein the rectification high-pressure tower T102NA is connected with the rectification low-pressure tower T102NB in parallel, the heat exchanger B9 is arranged between the two rectification towers, the tower top of the rectification tower T102NA is connected to a heat flow pipeline of the heat exchanger B9 to serve as a condensation cycle, the tower bottom of the rectification tower T102NB is connected to the inlet of a cold flow pipeline of the heat exchanger B9, the outlet of the cold flow pipeline of the heat exchanger B9 is connected to the lower part of the rectification tower T102NB to serve as a reboiling cycle, and a reflux pump is arranged on the cold flow pipeline.
GBL cocurrent flow multiple effect rectification process, comprising the following steps:
1) preheating a reacted GBL crude product (C-GBL) by a preheater B15N, feeding the GBL crude product (C-GBL) into the middle part of a negative pressure dehydration tower T101N, removing light boiling point (L-IMP) in the negative pressure dehydration tower T101N, distilling the light boiling point at the top of the negative pressure dehydration tower T101N, feeding the light boiling point into a THF (tetrahydrofuran) recovery process, and dividing a heavy component into two parts after flowing out from the bottom of the negative pressure dehydration tower T101N, and respectively feeding the two parts into a rectification high-pressure tower T102NA and a rectification low-pressure tower T102 NB;
2) distilling heavy components entering a negative pressure dehydration tower T101N of the rectification low pressure tower T102NB, collecting pure products (G-GBL) from the top of the tower, feeding bottom kettle liquid into a shell pass of a heat exchanger B9 from the bottom of the tower, evaporating and collecting the bottom kettle liquid serving as a cold material stream, returning the bottom kettle liquid to the upper part of a tower kettle of the rectification low pressure tower T102NB in a gas-liquid mixed state, and collecting a small amount of heavy components serving as reboil (H-GBL); at this time, the heat exchanger B9 serves as a reboiler of the rectification lower pressure column T102NB, and transfers heat from the rectification higher pressure column T102NA to the rectification lower pressure column T102 NB;
3) heavy components entering a negative pressure dehydration column T101N of the rectification high-pressure column T102NA are distilled, gas phase at the top of the rectification high-pressure column enters a heat exchanger B9 as a hot material stream to be condensed, the hot material stream leaves from the tube pass of the heat exchanger B9, part of solution is discharged as pure product under the pushing action of a reflux pump, part of solution flows back to the top of the rectification high-pressure column T102NA, kettle liquid discharged from the bottom of the rectification high-pressure column is discharged as reboiled, and at the moment, the heat exchanger B9 is used as a condenser of the rectification high-pressure column T102NA, absorbs heat from the top of the rectification high-pressure column T102NA and transfers the heat to the kettle of the rectification low-pressure column T102 NB;
4) the gas phase from the top of the rectification high-pressure tower T102NA is condensed by a heat exchanger B9 to obtain a pure product, and the pure product is converged with the pure product from the top of the rectification low-pressure tower T102NB and discharged out of the equipment as a final product.
In the process, Aspen Plus is utilized to simulate the GBL parallel-flow multi-effect rectification device, and by combining the graph shown in figure 3 and the table 3, the output flow of the GBL parallel-flow multi-effect rectification process is S15, the mass flow rate of the output flow is 3025kg/hr, the purity of the output flow is 99.86%, the original GBL rectification process is combined with the graph shown in figure 2 and the table 2, the output flow rate of the output flow is 133, the mass flow rate of the output flow is 3057kg/hr, the purity of the output flow is 99.78%, the output flow rate is converted into pure GBL, and the relative error is 0.0097.
TABLE 2 original GBL distillation recovery process stream table
TABLE 3 GBL cocurrent multiple effect rectification process stream table
On the basis, by combining fig. 3 and table 3, the energy consumption of the rectifying tower is compared, and as the evaporation intensity is highest when the temperature difference of cold and hot material flows is 30 ℃ during evaporation, as shown in table 4, it can be found that by adopting the parallel-flow multi-effect rectifying process of the invention, under the same technical index, the load of a condenser is reduced by 58.75% on the original basis, the load of a reboiler is reduced by 63.48%, and a good energy-saving effect is achieved.
TABLE 4 comparison table of GBL parallel flow multiple effect rectification process and original GBL rectification recovery process energy consumption
The GBL parallel-flow multi-effect rectification process has larger difference with the original GBL rectification process, the complex load of T102 is not simply divided into two parts of T102NA and T102NB, but the matching is carried out according to the cold-heat coupling of a high-pressure tower and a low-pressure tower, and the feeding and the yield of the two towers are different; because the operating pressure of the tower is different and the phase equilibrium constant is changed, in the invention, the pressure at the top of the rectification high-pressure tower T102NA is 20kPa, the pressure at the top of the rectification low-pressure tower T102NB is the same as that of the prior art and is 3kPa, in order to obtain the same product purity and meet the product quality after process adjustment, through calculation and verification, when the filler with the height of 0.5m is added, the product purity is higher than that of the prior art, namely, the theoretical stages of the rectification high-pressure tower T102NA are increased by 2, from 40 to 42, the total height of the tower is increased by 0.5m, and the rectification low-pressure tower T102NB is kept unchanged or is 40 theoretical stages. The feeding position of the rectification high-pressure column T102NA is that under the condition that the product yield is not changed, the heating quantity of the column bottom at different feeding positions is calculated step by taking the minimum heating quantity of the column bottom as an objective function, when the feeding position is 39 stages of column plates from the top of the column, the heating quantity of the column bottom is minimum, namely the optimal feeding position of the rectification high-pressure column T102NA is 39 stages of column plates from the top of the column, and the column parameters are shown in Table 5.
TABLE 5 comparison table of tower parameters of GBL parallel flow multiple effect rectification process and original GBL rectification recovery process
Further, the result of the hydraulic calculation of the rectification high-pressure column T102NA is shown in fig. 6, since the rectification column of the present invention is a pressurized column, a higher flooding rate needs to be selected, and when the flooding rate is set to 80%, the column diameter of the two tower plates (i.e., 1-26 stages) is required to be approximately 600mm, and the column diameter of the last tower plate (i.e., 27-41 stages) is required to be approximately 650mm, so that the column diameter of the rectification high-pressure column T102NA is taken to be 650mm according to the value of the standard column diameter; as a result of the hydraulic calculation of the rectifying low-pressure column T102NB, as shown in fig. 7, when the flooding ratio was set to 80%, the column diameter required was nearly 910mm, and therefore, the column diameter of the rectifying low-pressure column T102NB was taken to be 1000 mm.
Therefore, although the invention adopts two rectifying towers, the size of the tower is far smaller than that of the existing rectifying tower, the diameter of the tower is also far smaller than that of the existing rectifying tower, so that the using amount of the packing is also far smaller than that of the existing rectifying tower, the construction cost of the equipment is greatly reduced, and the consumption of manpower and material resources is reduced.
In the invention, the heat exchanger bears a tower top condenser of a rectification high-pressure tower T102NA and a tower bottom reboiler of a rectification low-pressure tower T102NB, absorbs heat from the tower top of the rectification high-pressure tower T102NA and transfers the heat to the tower bottom of the rectification low-pressure tower T102NB, compared with the prior art, under the same technical indexes, the load of the condenser is reduced by 58.75 percent on the original basis, the load of the reboiler is reduced by 63.48 percent, and A = Q/(. DELTA.T) is calculated by a simple method through simulationmU), where a is the heat transfer area, Q is the heat transfer amount, Δ TmIs the logarithmic mean temperature difference, U is the total heat transfer coefficient, as shown in FIG. 4, there is a temperature difference of 35-40 deg.C, divided from the heat transfer perspectiveAnd the heat transfer driving force of the heat exchanger B9 is larger, the required heat exchange area is smaller, and the resistance of the rectifying high-pressure tower T102NA can be reduced from the heat source analysis, so that the heating temperature of the heat load is reduced.
Further, as shown in FIG. 5, since the mean temperature difference of logarithmic heat transfer (LMTD) is large, the required heat exchange area is not so large, and is only 9.675m2And the method is easy to realize in engineering construction.
In summary, the GBL co-current multi-effect distillation apparatus and process method according to the present invention have been fully described with reference to the accompanying drawings by the preferred embodiments, and have the advantages of good energy saving effect, low construction cost, low construction difficulty, low consumption of manpower and material resources, and significant effect. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (4)
- GBL parallel flow multiple effect rectification process, characterized in that: the GBL parallel-flow multi-effect rectification device comprises a negative pressure dehydration tower and two rectification towers, wherein the two rectification towers are a rectification high-pressure tower (T102 NA) and a rectification low-pressure tower (T102 NB), the rectification high-pressure tower (T102 NA) and the rectification low-pressure tower (T102 NB) are connected in parallel, a heat exchanger (B9) is arranged between the rectification high-pressure tower (T102 NA) and the rectification low-pressure tower (T102 NB), the tower top of the rectification high-pressure tower (T102 NA) is connected to a heat flow tube pass of the heat exchanger (B9), the tower bottom of the low-pressure tower (T102 NB) is connected to a cold flow shell pass of the heat exchanger (B9), and a reflux pump is arranged on the cold flow shell pass;wherein: the theoretical stages of the rectification high-pressure tower (T102 NA) are 42, the diameter of the tower is 650mm, the theoretical stages of the rectification low-pressure tower (T102 NB) are 40, and the diameter of the tower is 1000 mm; the pressure at the top of the rectifying high-pressure column (T102 NA) is 20kPa, the pressure at the top of the rectifying low-pressure column (T102 NB) is 3kPa, the pressure drop of the rectifying high-pressure column (T102 NA) is 5kPa, and the pressure drop of the rectifying low-pressure column (T102 NB) is 3 kPa;the process comprises the following steps:1) preheating a reacted GBL crude product by a preheater (B15N), feeding the GBL crude product into the middle part of a negative pressure dehydration tower (T101N), removing light boiling in the negative pressure dehydration tower (T101N), distilling the light boiling at the top of the negative pressure dehydration tower (T101N), feeding the light boiling THF recovery procedure, and dividing a heavy component into two parts after flowing out from the bottom of the negative pressure dehydration tower (T101N) and feeding the two parts into a rectifying high-pressure tower (T102 NA) and a rectifying low-pressure tower (T102 NB) respectively;2) heavy components entering a negative pressure dehydration tower (T101N) of the rectification low pressure tower (T102 NB) are distilled, pure products are extracted from the top of the tower, bottom residue enters a shell pass of a heat exchanger (B9) from the bottom of the tower and is used as a cold material stream for evaporation and extraction, the cold material stream returns to the upper part of the tower bottom of the rectification low pressure tower (T102 NB) in a gas-liquid mixed state, and a small amount of the cold material stream is extracted as tar; at this time, the heat exchanger (B9) serves as a reboiler of the rectification lower pressure column (T102 NB) and transfers heat from the rectification higher pressure column (T102 NA) to the rectification lower pressure column (T102 NB);3) heavy components entering a negative pressure dehydration column (T101N) of the rectification high-pressure column (T102 NA) are distilled, gas phase at the top of the rectification high-pressure column enters a heat exchanger (B9) as a hot material stream to be condensed, the hot material stream leaves from the tube pass of the heat exchanger (B9), part of solution is discharged as a pure product under the pushing action of a reflux pump, part of solution flows back to the top of the rectification high-pressure column (T102 NA), kettle liquid discharged at the bottom of the rectification high-pressure column is discharged as reboiled, at the moment, the heat exchanger (B9) is used as a condenser of the rectification high-pressure column (T102 NA), heat from the top of the rectification high-pressure column (T102 NA) is absorbed, and the heat is transferred to the kettle of the rectification low-pressure column (T102 NB);4) the gas phase from the top of the rectification high-pressure tower (T102 NA) is condensed by a heat exchanger (B9) to obtain a pure product, and the pure product is merged with the pure product from the top of the rectification low-pressure tower (T102 NB) and discharged out of the equipment as a final product.
- 2. The GBL co-current multi-effect rectification process of claim 1 wherein: the feeding position of the rectification high-pressure column (T102 NA) is 39 stages from the top of the column, and the feeding position of the rectification low-pressure column (T102 NB) is the bottom of the column.
- 3. The GBL co-current multi-effect rectification process of claim 1 wherein: the reflux ratio of the rectification high-pressure column (T102 NA) is 0.48.
- 4. The GBL co-current multi-effect rectification process of claim 1 wherein: the heat exchange area of the heat exchanger (B9) is 9.675m2The inlet temperature of the heat flow tube pass of the heat exchanger is 147 ℃, and the inlet temperature of the cold flow shell pass of the heat exchanger is 102 ℃.
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