N-butanol purification system
By designing a positive butanol purification system, the method of combining the cycle and continuous operation combined with the distillation module solves the problem of low recycling efficiency in the complex and co -boiling system in the complex and co -boiling system, realizes high purity extraction and high recovery rate, and reduces energy consumption. Essence
Patent Information
- Application Number
- CN202421151484.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-23
- Publication Date
- 2025-01-24
- Estimated Expiration
- 2034-05-23
AI Technical Summary
The prior art is difficult to effectively recover high-purity n-butanol from complex azeotropic systems, and the separation efficiency is low and the recovery rate is not high.
A positive butanol purification system is designed. Through circulation and continuous operation, combined with orthopedly, the orthopedne sperm module, dehydration module, and orthopedic ether distillation module are used to use transformer distillation technology to achieve high -efficiency separation of materials.
It achieves high-purity extraction of n-butanol (purity reaches more than 99.8%) and increases recovery rate (more than 99%). At the same time, it reduces the pressure drop and tower still temperature, reduces the size of the tower, and saves energy and consumption.
Smart Images
Figure CN222384196U_ABST
Abstract
Description
Technical Field
[0001] The utility model provides a n-butanol purification system. Background Art
[0002] As an important fine chemical intermediate and chemical raw material, n-butanol has a wide range of applications. It can be used to manufacture n-butyl ester plasticizers of phthalic acid, aliphatic dibasic acids and phosphoric acid. It is also a raw material for making butyraldehyde, butyric acid, butylamine and butyl lactate in organic synthesis.
[0003] After the synthesis and purification of tributyl phosphate by n-butanol esterification, there will be a large amount of n-butanol solvent, including n-butanol, water, n-butyl ether and n-butyl chloride.
[0004] Since the substances in the mixture all have binary and ternary azeotropes with water, the separation of the system is difficult and the recovery rate is low. Utility Model Content
[0005] In order to overcome the defects in the prior art that it is difficult to recover n-butanol from a complex azeotropic system and it is difficult to obtain n-butanol with high purity; the utility model provides an n-butanol purification system, which separates materials by circulating and continuously operating, thereby improving separation efficiency and recovering high-purity n-butanol. Specifically, the extraction purity of n-butanol is above 99.8%, and the yield is above 99%; the system of the present application can further reduce the pressure drop and the bottom temperature of the tower during operation, reduce the size of the tower, and save energy and reduce consumption.
[0006] The utility model provides a n-butanol purification system, which comprises an n-butanol distillation module, a dehydration module and an n-butyl ether distillation module; the n-butanol distillation module comprises a first distillation tower, the tower top of the first distillation tower is provided with a first condensation circuit, and the first condensation circuit is provided with a first material outlet branch; the tower bottom of the first distillation tower is provided with a first reboiling circuit, and the first reboiling circuit is provided with an n-butanol outlet; the dehydration module comprises a second distillation tower, the feed inlet of the second distillation tower is connected to the first distillation tower through the first material outlet branch, the tower top of the second distillation tower is provided with a second condensation circuit, and the second condensation circuit is provided with a second material outlet branch; The bottom of the tower is provided with a second reboiling circuit, and the second reboiling circuit is provided with a water outlet; the n-butyl ether distillation module comprises a third distillation tower, the feed port of the third distillation tower is connected to the second distillation tower through the second material outlet branch, the top of the third distillation tower is provided with a third condensation circuit, and the third condensation circuit is respectively provided with a third material outlet branch and an n-butyl ether outlet; the bottom of the third distillation tower is provided with a third reboiling circuit, and the third reboiling circuit is provided with a fourth material outlet branch; the third distillation tower is connected to the feed port of the second distillation tower through the third material outlet branch, and the third distillation tower is also connected to the feed port of the first distillation tower through the fourth material outlet branch.
[0007] In the utility model, through the third material outlet branch and the fourth material outlet branch, the top material and the bottom material of the third distillation tower are respectively introduced into the second distillation tower and the first distillation tower to realize the circulation of materials; the distillation operation performed using the purification system belongs to pressure swing distillation.
[0008] In the utility model, the purification system of the present application can be used to purify n-butanol in n-butanol-water-n-butyl ether azeotrope.
[0009] In the utility model, the n-butyl ether-water-n-butyl alcohol azeotrope can be collected at the n-butyl ether outlet.
[0010] In some embodiments, the first condensation circuit and the second condensation circuit are each independently and sequentially provided with a condenser, a reflux tank and a pump.
[0011] In some embodiments, the third condensation circuit is provided with a condenser, a phase separator and a pump in sequence.
[0012] Wherein, in the third condensation circuit, a reflux tank may be provided between the condenser and the phase separator.
[0013] In some embodiments, the first reboiling loop, the second reboiling loop, and the third reboiling loop are each independently provided with a pump and a falling film reboiler; those skilled in the art should know that the falling film reboiler is an energy-saving device.
[0014] In some embodiments, the second condensation loop is connected to a heat exchange medium channel of a reboiler on the first reboiler loop, for providing heat of the second distillation tower top gas to the reboiler on the first reboiler loop.
[0015] In some embodiments, the first distillation tower, the second distillation tower, and the third distillation tower are all high-efficiency plate corrugated packing towers, which are packed in a regular manner and have the advantages of high separation efficiency and low pressure drop; if conventional packing methods or packed towers are used, there will be problems such as high pressure drop, high kettle temperature, and high energy consumption.
[0016] Among them, the parameters in the high-efficiency plate corrugated packing tower can be designed according to the equal plate height and pressure drop.
[0017] In one embodiment, the packing height of the high-efficiency plate corrugated packing tower is 6-12m.
[0018] Among them, those skilled in the art should know that the tower diameter of the high-efficiency plate corrugated packing tower is determined by the feed amount.
[0019] In some embodiments, the n-butanol purification system also includes a n-butyl chloride distillation module; the n-butyl chloride distillation module includes a fourth distillation tower, the top of the fourth distillation tower is provided with a fourth condensation loop, and the fourth condensation loop is provided with a n-butyl chloride outlet; the bottom of the first distillation tower is provided with a fourth reboiling loop, and the fourth reboiling loop is provided with a fifth material outlet branch; the fourth distillation tower is connected to the feed inlet of the first distillation tower through the fifth material outlet branch.
[0020] In the present invention, according to the name of the material or the function of the distillation tower, the fourth distillation tower can be called a light removal tower, the first distillation tower can be called a product tower, the second distillation tower can be called a dehydration tower, and the third distillation tower can be called a n-butyl ether tower.
[0021] The purification system containing the fourth distillation tower can be used to purify n-butanol in the azeotrope of n-butyl chloride-n-butanol-water-n-butyl ether.
[0022] Among them, the azeotropic product of n-butyl chloride-n-butyl alcohol-water-n-butyl ether can be collected at the outlet of n-butyl chloride.
[0023] In a preferred embodiment, the fourth condensation circuit is provided with a condenser, a phase separator and a pump in sequence.
[0024] Wherein, in the fourth condensation circuit, a reflux tank may be further provided between the condenser and the phase separator.
[0025] In a preferred embodiment, the fourth reboiler loop is provided with a pump and a falling film reboiler.
[0026] In a preferred embodiment, the fourth distillation tower is a high-efficiency plate corrugated packing tower; it is packed in a regular manner.
[0027] In one embodiment, the feed inlet of the first distillation tower is located in the middle of the first distillation tower; the feed inlet of the second distillation tower is located in the middle of the second distillation tower; the feed inlet of the third distillation tower is located in the middle of the third distillation tower; the feed inlet of the fourth distillation tower is located in the middle of the fourth distillation tower.
[0028] In the utility model, a method for purification using the n-butanol purification system comprises the following steps:
[0029] S1, the raw material enters the fourth distillation tower through the pump, the top liquid phase of the fourth distillation tower is extracted by the pump, and the bottom material of the fourth distillation tower is sent to the first distillation tower as feed;
[0030] S2, the overhead material of the first distillation tower enters the second distillation tower, and the first distillation tower kettle produces n-butanol product;
[0031] S3, the top gas of the second distillation tower is transported to the reboiler of the first distillation tower as a heat source, the top gas after condensation is sent to the third distillation tower, and the bottom gas of the second distillation tower is discharged into the wastewater that meets the discharge standards;
[0032] S4. The top of the third distillation tower is condensed and then transported to the second distillation tower or the n-butyl ether ternary azeotrope is produced, and the water phase in the bottom of the third distillation tower is transported to the first distillation tower.
[0033] Among them, the bottoms of the first distillation tower, the second distillation tower, the third distillation tower and the fourth distillation tower are all heated by 10 barg steam.
[0034] In the utility model, the heat in the condensing circuit and the reboiling circuit can use the public works with lower temperature as the heat source, so as to realize thermal coupling and low temperature, and achieve the effect of energy saving and consumption reduction.
[0035] On the basis of conforming to the common sense in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the present utility model.
[0036] The reagents and raw materials used in the utility model are all commercially available.
[0037] The positive and progressive effects of the utility model are:
[0038] (1) The purification system of the utility model separates materials by mixing different distillation technologies in a cyclic and continuous operation mode, thereby improving the separation efficiency and recovering high-purity n-butanol. Specifically, the extraction purity of n-butanol is above 99.8%, and its yield is above 99%;
[0039] (2) The system of the present application can further reduce the pressure drop and the tower temperature during operation, thereby reducing the size of the tower; and, by adopting a waste heat recovery method, the energy consumption of the system is reduced. BRIEF DESCRIPTION OF THE DRAWINGS
[0040] Figure 1 This is the n-butanol purification system of Example 1 of the utility model.
[0041] Description of reference numerals:
[0042] Butanol distillation module 1
[0043] The first distillation tower 101
[0044] The first condensation circuit 102
[0045] First material outlet branch 103
[0046] The first reboiler circuit 104
[0047] Butanol export 105
[0048] Dehydration module 2
[0049] The second distillation tower 201
[0050] Second condensation circuit 202
[0051] Second material outlet branch 203
[0052] Second reboiler loop 204
[0053] Water outlet 205
[0054] Butyl ether distillation module 3
[0055] The third distillation tower 301
[0056] The third condensation circuit 302
[0057] The third material outlet branch 303
[0058] n-Butyl ether export 304
[0059] The third reboiler circuit 305
[0060] Fourth material outlet branch 306
[0061] Chlorobutyl distillation module 4
[0062] Fourth distillation tower 401
[0063] Fourth condensation circuit 402
[0064] n-Butyl Chloride Export 403
[0065] Fourth reboiler loop 404
[0066] Fifth material outlet branch 405 . DETAILED DESCRIPTION
[0067] The present invention is further described below by way of examples, but the present invention is not limited to the scope of the examples. The experimental methods without specific conditions in the following examples are selected according to conventional methods and conditions, or according to the product specifications.
[0068] Example 1
[0069] This embodiment discloses a n-butanol purification system. Figure 1 This is the n-butanol purification system of this embodiment.
[0070] The n-butanol purification system comprises a n-butyl chloride distillation module 4, a n-butanol distillation module 1, a dehydration module 2 and a n-butyl ether distillation module 3; the n-butanol distillation module 1 comprises a first distillation tower 101, a first condensation circuit 102 is provided at the top of the first distillation tower 101, and a first material outlet branch 103 is provided on the first condensation circuit 102; a first reboiling circuit 104 is provided at the bottom of the first distillation tower 101, and a n-butanol outlet 105 is provided on the first reboiling circuit 104; the dehydration module 2 comprises a second distillation tower 201, a feed inlet of the second distillation tower 201 is connected to the first distillation tower 101 through the first material outlet branch 103, a second condensation circuit 202 is provided at the top of the second distillation tower 201, and a second material outlet branch 203 is provided on the second condensation circuit 202; a bottom of the second distillation tower 201 A second reboiling loop 204 is provided, and a water outlet 205 is provided on the second reboiling loop 204; the n-butyl ether distillation module 3 includes a third distillation tower 301, and the feed port of the third distillation tower 301 is connected to the second distillation tower 201 through a second material outlet branch 203, and a third condensation loop 302 is provided at the top of the third distillation tower 301, and a third material outlet branch 303 and an n-butyl ether outlet 304 are respectively provided on the third condensation loop 302; a third reboiling loop 305 is provided at the bottom of the third distillation tower 301, and a fourth material outlet branch 306 is provided on the third reboiling loop 305; the third distillation tower 301 is connected to the feed port of the second distillation tower 201 through the third material outlet branch 303, and the third distillation tower 301 is also connected to the feed port of the first distillation tower 101 through the fourth material outlet branch 306. The n-butyl chloride distillation module 4 includes a fourth distillation tower 401, a fourth condensation loop 402 is provided at the top of the fourth distillation tower 401, and a n-butyl chloride outlet 403 is provided on the fourth condensation loop 402; a fourth reboiling loop 404 is provided at the bottom of the first distillation tower 101, and a fifth material outlet branch 405 is provided on the fourth reboiling loop 404; the fourth distillation tower 401 is connected to the feed port of the first distillation tower 101 through the fifth material outlet branch 405.
[0071] Among them, the first condensation circuit 102 and the second condensation circuit 202 are independently and sequentially provided with a condenser, a reflux tank and a pump; the third condensation circuit 302 and the fourth condensation circuit 402 are independently and sequentially provided with a condenser, a phase separator and a pump; the first reboiler circuit 104, the second reboiler circuit 204, the third reboiler circuit 305 and the fourth reboiler circuit 404 are independently provided with a pump and a falling film reboiler. The second condensation circuit 202 is connected to the heat exchange medium channel of the reboiler on the first reboiler circuit 104, and is used to provide the heat of the top gas of the second distillation tower 201 to the reboiler on the first reboiler circuit 104. The first distillation tower 101, the second distillation tower 201, the third distillation tower 301 and the fourth distillation tower 401 are all high-efficiency plate corrugated packing towers, which are packed in a regular manner. The packing height of the high-efficiency plate corrugated packing tower is 10m. The feed inlet of the first distillation tower 101 is located in the middle of the first distillation tower 101; the feed inlet of the second distillation tower 201 is located in the middle of the second distillation tower 201; the feed inlet of the third distillation tower 301 is located in the middle of the third distillation tower 301; the feed inlet of the fourth distillation tower 401 is located in the middle of the fourth distillation tower 401.
[0072] The purification system of this embodiment is used to purify n-butanol in the azeotrope of n-butyl chloride-n-butanol-water-n-butyl ether.
[0073] Example 2
[0074] This embodiment discloses a purification method using the n-butanol purification system of embodiment 1, which comprises the following steps:
[0075] S1, the raw material enters the fourth distillation tower 401 through the pump, the top liquid phase of the fourth distillation tower 401 is extracted by the pump, and the extracted material from the bottom of the fourth distillation tower 401 is sent to the first distillation tower 101 as feed;
[0076] S2, the top material of the first distillation tower 101 enters the second distillation tower 201, and the bottom of the first distillation tower 101 produces n-butanol product;
[0077] S3, the top gas of the second distillation tower 201 is transported to the reboiler of the bottom of the first distillation tower 101 as a heat source, the top gas after condensation is sent to the third distillation tower 301, and the bottom gas of the second distillation tower 201 is discharged into the wastewater meeting the discharge standards;
[0078] S4. The top of the third distillation tower 301 is condensed and then transported to the second distillation tower 201 or the n-butyl ether ternary azeotrope is produced, and the water phase in the bottom of the third distillation tower 301 is transported to the first distillation tower 101.
[0079] The composition of the raw material is: 2wt% of n-butyl chloride, 15wt% of water, 82.49wt% of n-butanol, 0.5wt% of n-butyl ether, and 0.01wt% of tributyl phosphate; the process conditions when it enters the fourth distillation tower are as follows: temperature is 30°C, pressure is 3000mbara (mbara refers to absolute pressure), and feed flow rate is 6000kg / h.
[0080] Table 1 shows the produced materials at each outlet after purification by the n-butanol purification system of Example 1.
[0081] Table 1
[0082]
[0083] According to the data recorded in Table 1, the purity of n-butanol in the produced material at the n-butanol export is above 99.8%, and according to the calculation formula of the yield:
[0084] Ethanol yield = (content of n-butanol in n-butanol outlet material × material flow rate of n-butanol outlet) / (content of n-butanol in raw material × feed flow rate)
[0085] The yield of n-butanol was calculated to be over 99%.
Claims
1. A n-butanol purification system, characterized in that: It includes a n-butanol distillation module, a dehydration module and a n-butyl ether distillation module; The n-butanol distillation module comprises a first distillation tower, the top of which is provided with a first condensation circuit, and the first condensation circuit is provided with a first material outlet branch; the bottom of the first distillation tower is provided with a first reboiling circuit, and the first reboiling circuit is provided with an n-butanol outlet; The dehydration module comprises a second distillation tower, the feed inlet of the second distillation tower is connected to the first distillation tower through the first material outlet branch, the top of the second distillation tower is provided with a second condensation circuit, and the second condensation circuit is provided with a second material outlet branch; the bottom of the second distillation tower is provided with a second reboiling circuit, and the second reboiling circuit is provided with a water outlet; The n-butyl ether distillation module includes a third distillation tower, the feed port of the third distillation tower is connected to the second distillation tower through the second material outlet branch, the top of the third distillation tower is provided with a third condensation circuit, and the third condensation circuit is respectively provided with a third material outlet branch and an n-butyl ether outlet; the bottom of the third distillation tower is provided with a third reboiling circuit, and the third reboiling circuit is provided with a fourth material outlet branch; the third distillation tower is connected to the feed port of the second distillation tower through the third material outlet branch, and the third distillation tower is also connected to the feed port of the first distillation tower through the fourth material outlet branch.
2. The n-butanol purification system according to claim 1, characterized in that: The first condensation circuit and the second condensation circuit are independently and sequentially provided with a condenser, a reflux tank and a pump; The third condensation circuit is provided with a condenser, a phase separator and a pump in sequence.
3. The n-butanol purification system according to claim 1, characterized in that: The first reboiling circuit, the second reboiling circuit and the third reboiling circuit are each independently provided with a pump and a falling film reboiler.
4. The n-butanol purification system according to claim 1, characterized in that: The second condensation circuit is connected to the heat exchange medium channel of the reboiler on the first reboiler circuit, and is used to provide the heat of the top gas of the second distillation tower to the reboiler on the first reboiler circuit.
5. The n-butanol purification system according to claim 1, characterized in that: The first distillation tower, the second distillation tower and the third distillation tower are all high-efficiency plate corrugated packing towers.
6. The n-butanol purification system according to claim 1, characterized in that: The n-butanol purification system also includes a n-butyl chloride distillation module; The n-butyl chloride distillation module comprises a fourth distillation tower, a fourth condensation loop is provided at the top of the fourth distillation tower, and a n-butyl chloride outlet is provided on the fourth condensation loop; a fourth reboiler loop is provided at the bottom of the first distillation tower, and a fifth material outlet branch is provided on the fourth reboiler loop; the fourth distillation tower is connected to the feed port of the first distillation tower via the fifth material outlet branch.
7. The n-butanol purification system according to claim 6, characterized in that: The fourth condensation circuit is provided with a condenser, a phase separator and a pump in sequence.
8. The n-butanol purification system according to claim 6, characterized in that: The fourth reboiler loop is provided with a pump and a falling film reboiler.
9. The n-butanol purification system according to claim 6, characterized in that: The fourth distillation tower is a high-efficiency plate corrugated packing tower.
10. The n-butanol purification system according to any one of claims 6 to 9, characterized in that: The feed inlet of the first distillation tower is arranged in the middle of the first distillation tower; The feed inlet of the second distillation tower is arranged in the middle of the second distillation tower; The feed inlet of the third distillation tower is arranged in the middle of the third distillation tower; The feed inlet of the fourth distillation tower is arranged in the middle of the fourth distillation tower.