CN117065379B - Separation device for purifying BDO from BDO waste liquid - Google Patents

Separation device for purifying BDO from BDO waste liquid Download PDF

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CN117065379B
CN117065379B CN202311343328.9A CN202311343328A CN117065379B CN 117065379 B CN117065379 B CN 117065379B CN 202311343328 A CN202311343328 A CN 202311343328A CN 117065379 B CN117065379 B CN 117065379B
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bdo
evaporator
distribution plate
tower
evaporation
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CN117065379A (en
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黄惠珊
陈惠燕
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Fujian Juchuangxin Material Technology Co ltd
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Fujian Juchuangxin Material Technology Co ltd
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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
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/30—Accessories for evaporators ; Constructional details thereof
    • 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
    • B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
    • 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
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/36—Azeotropic distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/28—Moving reactors, e.g. rotary drums
    • B01J19/285—Shaking or vibrating reactors; reactions under the influence of low-frequency vibrations or pulsations
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F22—STEAM GENERATION
    • F22B—METHODS OF STEAM GENERATION; STEAM BOILERS
    • F22B1/00—Methods of steam generation characterised by form of heating method
    • F22B1/22—Methods of steam generation characterised by form of heating method using combustion under pressure substantially exceeding atmospheric pressure
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G5/00—Incineration of waste; Incinerator constructions; Details, accessories or control therefor
    • F23G5/44—Details; Accessories
    • F23G5/46—Recuperation of heat
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/04—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste liquors, e.g. sulfite liquors

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Combustion & Propulsion (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention relates to the technical field of separation devices, in particular to a separation device for purifying BDO from BDO waste liquid. The separating device for purifying BDO from BDO waste liquid comprises an evaporating mechanism and a combustion mechanism, wherein a first condenser is connected to the evaporating mechanism, a separating mechanism for separating BDO residual liquid is connected to a discharge port of the first condenser, an oxidation reaction mechanism is connected to a discharge port of the separating mechanism, and a rectifying mechanism is arranged on a discharge port of the oxidation reaction mechanism; the combustion mechanism is respectively connected with the evaporation mechanism and the rectification mechanism and is used for receiving the tailings of the evaporation mechanism and the rectification mechanism and burning the tailings to provide heat for the evaporation mechanism and the rectification mechanism, so that the full utilization of waste liquid resources is realized, and secondary pollution emission of waste water, waste gas, waste solids and the like is avoided, and the environment is protected.

Description

Separation device for purifying BDO from BDO waste liquid
Technical Field
The invention relates to the technical field of separation devices, in particular to a separation device for purifying BDO from BDO waste liquid.
Background
1, 4-butanediol (BDO for short) is an important chemical raw material, is a raw material for producing high-end fine chemical products, and is mainly used for producing products such as polybutylene terephthalate (PBT), gamma-butyrolactone (GBL), N-methylpyrrolidone, tetrahydrofuran (THF), polytetramethylene ether glycol (PTMEG), polyurethane and the like. The existing 1, 4-butanediol production process mainly comprises an alkynal method, a maleic anhydride method, a butadiene method, a propylene oxide method and the like. In the BDO production processes, in order to obtain BDO finished products with qualified purity and chromaticity, waste liquid is required to be discharged from the tower bottom periodically in the BDO separation, purification and refining process, however, the residual BDO content in the waste liquid is often between 20 and 40 percent, so that how to separate and recycle BDO in the waste liquid has higher application value.
Because the main components of the BDO-containing raffinate are low carbon chain alcohol, water, ethers, BDO, high polymers and salts, and the BDO raffinate mainly comes from the bottom of a BDO purification refining tower, the polymer and the salts in the material are high in content and high in viscosity, so that the evaporation efficiency is low and the BDO yield is low in the traditional raffinate separation and recovery process, and is generally only 30-40%; meanwhile, the chromaticity of BDO recovered by separation does not reach the standard, so that the downstream product use is seriously affected, and the BDO cannot be sold as a finished product BDO. The BDO residual liquid is basically used as waste liquid for incineration treatment in the traditional process, so that serious waste of resources is caused.
Therefore, at present, the purity of BDO obtained by the separating device for purifying BDO from waste liquid for producing BDO and whether the purity meets national standard requirements are not described; meanwhile, the existing BDO separating device can not realize negative energy consumption production, and the separating and purifying process of the BDO separating device needs to consume relatively large energy, so that the separating and recycling cost of the BDO separating device is far greater than the cost of burning waste liquid.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a separating device for purifying BDO from BDO waste liquid.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the separating device for purifying BDO from BDO waste liquid comprises an evaporating mechanism and a combustion mechanism, wherein the evaporating mechanism comprises an evaporator, a stirring assembly for accelerating liquid evaporation is arranged on the evaporator, a first condenser is connected to a discharge port of the evaporator, a separating mechanism for separating BDO residual liquid is connected to the discharge port of the first condenser, and an oxidation reaction mechanism is connected to the discharge port of the separating mechanism;
the oxidation reaction mechanism comprises an oscillation generator, the output end of the oscillation generator is connected with a feeding section, the discharge port of the feeding section is connected with a reactor main body, the reactor main body comprises a reaction tank body, a liquid distribution plate is arranged in the reaction tank body, a plurality of uniformly distributed water cap holes are formed in the liquid distribution plate, and water caps are detachably connected to the water cap holes;
a rectifying mechanism is arranged on a discharge hole of the reactor main body;
the combustion mechanism comprises a combustion boiler which is respectively connected with the evaporation mechanism and the rectification mechanism and is used for receiving the tailings of the evaporation mechanism and the rectification mechanism and burning the tailings to provide heat for the evaporation mechanism and the rectification mechanism.
Further, the evaporator comprises an evaporation tank body, the stirring assembly is arranged on the evaporation tank body, the stirring assembly comprises a motor bracket arranged on the evaporation tank body, the middle part of the motor bracket is connected with a motor, the bottom of the motor is connected with a rotating shaft, and the upper part of the rotating shaft is connected with a first liquid distributor; the lower part of axis of rotation is connected with the connecting plate, the both ends of connecting plate are equipped with the scraper blade, the internal connection of scraper blade has the puddler, the puddler keep away from the one end of scraper blade with axis of rotation welded connection.
Further, the top of the evaporating pot body is provided with a feed inlet and an exhaust port respectively at two sides of the motor bracket; the right side of the bottom of the evaporating pot body is connected with a circulating pump, the top of the circulating pump is connected with a guide pipe, and a discharge hole of the guide pipe is communicated with the first liquid distributor.
Further, the evaporator comprises a first evaporator and a second evaporator, wherein a discharge port of the first evaporator is connected with a material pumping pump, and a discharge port of the material pumping pump is communicated with a feed inlet of the second evaporator; the exhaust port of the second evaporator is communicated with the first condenser, the exhaust port of the first evaporator is connected with the second condenser, and the second condenser is communicated with the combustion mechanism.
Further, the first condenser and/or the second condenser comprises a condensing chamber I, a condensing pipe I is arranged in the condensing chamber I, and the condensing pipe I is in a spiral structure.
Further, the separating mechanism comprises a layered cavity, a drainage control assembly is arranged at the bottom of the layered cavity, a drainage tube is connected to the output end of the drainage control assembly, a discharge hole of the drainage tube is connected with the oxidation reaction mechanism, a siphon is arranged on the layered cavity, and the other end of the siphon is communicated with the second evaporator.
Further, the liquid distribution plate comprises a first distribution plate, a second distribution plate and a third distribution plate which are arranged in the tank body from top to bottom in sequence, the diameter of the second distribution plate is larger than that of the first distribution plate or the third distribution plate, and the diameters of the first distribution plate and the third distribution plate are equal; and a packing layer is arranged among the first distribution plate, the second distribution plate and the third distribution plate, and random packing made of ceramic materials or glass materials is filled in the packing layer.
Further, the top and the bottom of the reaction tank body are respectively provided with a first end cover and a second end cover, the first end cover is provided with a discharge hole, the second end cover is provided with a feed inlet matched with the feed section, and the feed inlet is provided with a second liquid distributor.
Further, the rectifying mechanism comprises a rectifying tower, a third condensing mechanism is arranged at the bottom of the rectifying tower and comprises a condensing chamber II, a condensing pipe II is arranged in the condensing chamber II, and the other end of the condensing pipe II extends to the outer side of the right lower end of the condensing chamber II; the rectifying tower is characterized in that a tower plate assembly is arranged inside the rectifying tower and is formed by sequentially and alternately arranging annular tower plates and circular tower plates up and down, the annular tower plates and the circular tower plates are horizontally arranged, the annular tower plates are arranged on the tower wall of the rectifying tower, and the circular tower plates are connected with the tower wall of the rectifying tower through connecting rods.
Further, the rectifying tower comprises a first rectifying tower and a second rectifying tower, a condensing chamber III is connected to an exhaust port of the first rectifying tower, a condensing pipe III is installed in the condensing chamber III, and the other end of the condensing pipe III is communicated with a feed inlet of the combustion mechanism; the condenser pipe II that first rectifying column bottom was established with the feed inlet of second rectifying column is linked together, be connected with condensation chamber IV on the gas vent of second rectifying column, install condensation pipe IV in the condensation chamber IV, condensation chamber IV's lower extreme fixedly connected with row material pipe, condensation pipe IV's lower extreme with arrange the upper end of material pipe and put through each other, connect the material bottle is installed to row material pipe's tip.
As can be seen from the above description of the present invention, compared with the prior art, the present invention has the following advantages: 1. according to the invention, by arranging the evaporation mechanism, the combustion mechanism, the first condenser, the separation mechanism, the oxidation reaction mechanism and the rectification mechanism, waste liquid resources can be fully utilized, and secondary pollution emission such as waste water, waste gas, waste solid and the like is avoided, so that the device is environment-friendly.
2. The evaporating mechanism comprises a first evaporator and a second evaporator, so that polymers and salts in BDO residual liquid can be effectively removed, and the entrainer is added in the second evaporator, so that BDO can be brought out of the BDO residual liquid in an azeotropic manner by utilizing strong action force or similar relative volatility between the entrainer and BDO, and the BDO and the entrainer can be removed with low energy consumption after being condensed, thereby obtaining a BDO finished product. Meanwhile, the viscosity of BDO raffinate is effectively reduced in the azeotropic distillation process, the BDO yield is improved, the recovery rate can reach 85-95%, and the total recovery rate is higher than 80% of the total recovery rate of directly recovering distilled waste liquid in the industry at present.
3. According to the invention, by arranging the oxidation reaction mechanism, some unsaturated chromophoric substances in BDO residual liquid are converted into colorless substances, and then the colorless substances are coupled with rectification, so that the chromaticity of BDO finished products meets the national standard requirements.
4. The combustion mechanism disclosed by the invention combines the residues from BDO removal with light components in the BDO crude product obtained by rectification and then burns, and the heat value of the material is 5500-6000kcal/kg, so that steam generated by material combustion is used for supplying steam required by a BDO purification section, and BDO in the purified residual liquid with negative energy consumption is realized.
Drawings
FIG. 1 is a schematic structural diagram of a separation device for purifying BDO from BDO waste liquid in a preferred embodiment of the invention;
FIG. 2 is a schematic view showing the structure of an evaporator according to a preferred embodiment of the present invention;
FIG. 3 is a schematic view of a separating mechanism according to a preferred embodiment of the present invention;
FIG. 4 is a schematic view showing the structure of an oxidation reaction mechanism according to a preferred embodiment of the present invention;
FIG. 5 is a schematic view showing the structure of a first rectifying column in a preferred embodiment of the present invention;
FIG. 6 is a schematic diagram showing the structure of a second rectifying tower according to the preferred embodiment of the present invention;
reference numerals: 1. an evaporation mechanism; 100. an evaporator; 100a, a first evaporator; 100b, a second evaporator;
101. an evaporation tank body; 102. a motor bracket; 103. a motor; 104. a rotating shaft; 105. a first liquid distributor; 106. a connecting plate; 107. a scraper; 108. a stirring rod; 109. a feed inlet; 110. an exhaust port; a 111 circulation pump; 112. a conduit; 113. a material pump;
2. a combustion mechanism; 3. a first condenser;
4. a separation mechanism;
401. a layered cavity; 402. a drainage control assembly; 403. a drainage tube; 404. a siphon tube;
5. an oxidation reaction mechanism;
501. an oscillation generator; 502. a feed section; 503. a reactor body; 504. a liquid distribution plate; 505. a first end cap; 506. a second end cap; 507. a second liquid distributor;
6. a rectifying mechanism; 600. a rectifying tower; 600a, a first rectifying tower; 600b, a second rectifying tower;
601. a condensing chamber II; 602. a condensing tube II; 603. a tray assembly; 604. a condensation chamber III; 605. a condenser tube III; 606. a condensing chamber IV; 607. a condensing tube IV; 608. a discharge pipe; 609. a receiving bottle;
7. and a second condenser.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention.
Referring to fig. 1-6, a separation device for purifying BDO from BDO waste liquid according to a preferred embodiment of the present invention comprises an evaporation mechanism 1 and a combustion mechanism 2, wherein the evaporation mechanism 1 comprises an evaporator 100, a stirring assembly for accelerating evaporation of liquid is installed on the evaporator 100, a first condenser 3 is connected to a discharge port of the evaporator 100, a separation mechanism 4 for separating BDO residual liquid is connected to a discharge port of the first condenser 3, and an oxidation reaction mechanism 5 is connected to a discharge port of the separation mechanism 4;
the oxidation reaction mechanism 5 comprises an oscillation generator 501, the output end of the oscillation generator 501 is connected with a feeding section 502, a discharge port of the feeding section 502 is connected with a reactor main body 503, the reactor main body 503 comprises a reaction tank body, a liquid distribution plate 504 is arranged in the reaction tank body, a plurality of uniformly distributed water cap holes are formed in the liquid distribution plate 504, and water caps are detachably connected to the water cap holes; a rectifying mechanism 6 is arranged on the discharge hole of the reactor main body;
the combustion mechanism 2 comprises a combustion boiler which is respectively connected with the evaporation mechanism 1 and the rectification mechanism 6 and is used for receiving the tailings of the evaporation mechanism 1 and the rectification mechanism 6 and burning the tailings to provide heat for the evaporation mechanism 1 and the rectification mechanism 6, so that the full utilization of waste liquid resources is realized, secondary pollution emission such as no waste water, waste gas, waste solid and the like is avoided, and the combustion mechanism is environment-friendly.
As a preferred embodiment of the invention, it may also have the following additional technical features: the evaporator 100 comprises an evaporation tank body 101, the stirring assembly is arranged on the evaporation tank body 101, the stirring assembly comprises a motor bracket 102 arranged on the evaporation tank body 101, a motor 103 is connected to the middle of the motor bracket 102, a rotating shaft 104 is connected to the bottom of the motor 103, and a first liquid distributor 105 is connected to the upper part of the rotating shaft 104; the lower part of axis of rotation 104 is connected with connecting plate 106, the both ends of connecting plate 106 are equipped with scraper blade 107, the internal connection of scraper blade 107 has puddler 108, the puddler 108 keep away from the one end of scraper blade 107 with axis of rotation 104 welded connection. Therefore, the uniform heating of the raw materials is realized, and the evaporation progress of the raw materials is quickened.
In this embodiment, the top of the evaporation tank 101 is located at two sides of the motor bracket 102, and a feed inlet 109 and an exhaust outlet 110 are respectively provided; the right side of the bottom of the evaporation tank 101 is connected with a circulating pump 111, the top of the circulating pump 111 is connected with a conduit 112, and a discharge port of the conduit 112 is communicated with the first liquid distributor 105. Thereby enabling the feedstock to be fully vaporized, resulting in higher recovery and higher purity BDO.
In this embodiment, the evaporator 100 includes a first evaporator 100a and a second evaporator 100b, a discharge port of the first evaporator 100a is connected to a material pump 113, and a discharge port of the material pump 113 is communicated with a feed port of the second evaporator 100 b; the exhaust port of the second evaporator is communicated with the first condenser 3, the exhaust port of the first evaporator 100a is connected with a second condenser 7, and the second condenser 7 is communicated with the combustion mechanism 2; the second evaporator 100b is an azeotropic evaporator. Therefore, the entrainer can be added into the second evaporator 100b, so that the BDO in the evaporated vapor phase can be discharged together with the entrainer by utilizing the strong action force between the entrainer and the BDO, and the recovery rate of the BDO reaches 85-95 percent; simultaneously, the viscosity of BDO raffinate can be reduced by adding the entrainer, so that BDO can be more easily carried out of the raffinate in an azeotropic mode.
In this embodiment, the first condenser 3 and the second condenser 7 include a condensation chamber I, in which a condensation tube I is installed, and the condensation tube I has a spiral structure. Therefore, steam can be quickly condensed, liquid with heat is transmitted to the liquid storage tank on the combustion mechanism through the pipeline by the condensing chamber, the liquid in the liquid storage tank obtains heat in fuel combustion and boils, liquid vapor is transmitted by the pipeline for the evaporation mechanism and the rectifying mechanism to work, and meanwhile, the liquid condensed by the evaporation mechanism and the rectifying mechanism is transmitted to the condensing chamber of the condenser through the pipeline to condense materials in the condensing pipe, so that energy recycling and full utilization are realized.
In this embodiment, the combustion mechanism 2 further includes a steam generator connected to the combustion boiler, so that the tails of the evaporation mechanism 1 and the rectification mechanism 6 burn in the combustion boiler to generate a large amount of high-temperature and high-pressure steam (the temperature is about 540 ℃, the pressure is about 9.8 MP), and the steam generator is used for performing the work of reducing temperature and reducing pressure to output clean power, and meanwhile, the reduced-temperature and reduced-pressure steam (the temperature is about 340 ℃, the pressure is about 3.8 MP) is connected to a public pipeline to provide heat for the evaporation mechanism 1 and the rectification mechanism 6, and the whole separation device is self-contained and is used for eating, squeezing, clean and zero emission.
In this embodiment, the separation mechanism 4 includes a layered cavity 401, a drainage control assembly 402 is disposed at the bottom of the layered cavity 401, an output end of the drainage control assembly 402 is connected with a drainage tube 403, a discharge port of the drainage tube 403 is connected with the oxidation reaction mechanism 5, a siphon 404 is mounted on the layered cavity 401, and the other end of the siphon 404 is communicated with the second evaporator 100 b. Therefore, the entrainer can be separated from BDO, and BDO with higher purity is obtained; and the azeotropic agent can be recycled through the arrangement of the siphon, so that the waste of raw materials is effectively avoided.
In this embodiment, the liquid distribution plate 504 includes a first distribution plate, a second distribution plate, and a third distribution plate that are installed in the tank body and sequentially arranged from top to bottom, where the diameter of the second distribution plate is greater than that of the first distribution plate or the third distribution plate, and the diameters of the first distribution plate and the third distribution plate are equal; and a packing layer is arranged among the first distribution plate, the second distribution plate and the third distribution plate, and random packing made of ceramic materials or glass materials is filled in the packing layer. Therefore, the method can fully react with the oxidant to ensure that some unsaturated chromophoric substances in BDO residual liquid are converted into colorless substances, and ensures that the purity of the rectified BDO reaches more than 99.5 percent.
In this embodiment, the top and the bottom of the reaction tank body are respectively provided with a first end cover 505 and a second end cover 506, a discharge port is provided on the first end cover 505, a feed port adapted to the feed section 502 is provided on the second end cover 506, and a second liquid distributor 507 is provided on the feed port. Thus, the contact area of the raw materials can be increased, so that the raw materials can be sufficiently reacted.
In this embodiment, the rectifying mechanism 6 includes a rectifying tower 600, a condensation chamber II601 is disposed at the bottom of the rectifying tower 600, a condensation pipe II602 is installed in the condensation chamber II601, and the other end of the condensation pipe II602 extends to the outer side of the right lower end of the condensation chamber II 601; the inside tray subassembly 603 that is equipped with of rectifying column 600, the tray subassembly comprises annular column tray and circular column tray upper and lower alternate arrangement in proper order, annular column tray and circular column tray all level set up, annular column tray is established on the tower wall of rectifying column, circular column tray pass through the connecting rod with the tower wall of rectifying column links to each other. Therefore, the raw materials can fully react, and the purity of the BDO obtained by rectification is ensured to be more than 99.5 percent.
In this embodiment, the rectifying tower 600 includes a first rectifying tower 600a and a second rectifying tower 600b, a condensation chamber III604 is connected to an exhaust port of the first rectifying tower 600a, a condensation pipe III605 is installed in the condensation chamber III604, and the other end of the condensation pipe III605 is communicated with a feed inlet of the combustion mechanism 2; the condenser pipe II that first rectifying column 600a bottom was established with the feed inlet of second rectifying column 600b is linked together, be connected with condensation chamber IV606 on the gas vent of second rectifying column 600b, install condenser pipe IV607 in the condensation chamber IV606, the lower extreme fixedly connected with of condensation chamber IV606 arranges material pipe 608, the lower extreme of condenser pipe IV607 with arrange the upper end of material pipe 608 and put through each other, connect the material bottle 609 is installed to the tip of arranging material pipe 608. Therefore, BDO is refined, and BDO products with qualified chromaticity are obtained, and the BDO products accord with international standards.
The working principle of the invention is as follows: 5kg of 30% BDO raffinate is put into a first evaporator for evaporation, the feed liquid of the first evaporator 100a is pumped into a second evaporator 100b through a material pump 113 for azeotropic evaporation, condensation is carried out under the action of a first condenser 3, BDO liquid and entrainer are separated by a separation mechanism 4, and the separated BDO liquid enters a rectification mechanism 6 for rectification, so that BDO products with qualified chromaticity are obtained, and the results are shown in Table 1.
TABLE 1
Name of the name First evaporator feed Layered tank discharging Discharging material of first rectifying tower kettle Side line discharging of second rectifying tower
Material/kg 5 1.53 1.43 1.08
BDO/wt% 30 83 89.2 99.5
The BDO products obtained by the separation device are subjected to a chromaticity test, and the tailings are subjected to a combustion test, and the result is as follows.
1. Colorimetric test
By detecting BDO products before oxidation and BDO products obtained through rectification after oxidation by adopting a colorimeter, the chromaticity of the BDO products before oxidation is about 30, the chromaticity of the BDO products obtained through rectification after oxidation is 0-5, and the chromaticity international standard of the BDO products is 0-10 at present, so that the BDO products prepared by the device of the application meet the international standard.
2. Tailing burning test
TABLE 2
Therefore, on the one hand, the invention aims at the problem of low yield, creatively utilizes the azeotropic distillation technology, utilizes the strong action force between the entrainer and BDO by adding the entrainer into the BDO raffinate, simultaneously reduces the viscosity of the BDO raffinate by adding the entrainer, brings BDO out of the raffinate by an azeotropic way, and the yield of BDO in the raffinate can reach 85-95%.
On the other hand, aiming at the problem of unqualified chromaticity, the method is coupled with a rectification technology through oxidation treatment, an oxidation reactor is combined, some unsaturated chromophoric substances in BDO raffinate are converted into colorless substances through oxidation reaction, and then the rectification separation technology is combined, so that the purity of BDO reaches more than 99.5%, the BDO is refined, and a BDO product with qualified chromaticity is obtained, and meets the international standard.
By implementing the device, the separation process with negative energy consumption of BDO is realized. After the residue from BDO separation is combined with light components in the BDO crude product obtained by rectification, the heat value of the material is about 5500-6000kcal/kg, steam generated by material combustion is used for supplying steam required by a BDO purification working section, BDO in the purified residual liquid with negative energy consumption is realized, zero emission of BDO separation is realized, the environmental protection benefit is very obvious, the production cost is effectively reduced, and the production benefit is improved.
The above additional technical features can be freely combined and superimposed by a person skilled in the art without conflict.
It will be understood that the invention has been described in terms of several embodiments, and that various changes and equivalents may be made to these features and embodiments by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (6)

1. Separation device of purification BDO in follow BDO waste liquid, its characterized in that: the device comprises an evaporation mechanism and a combustion mechanism, wherein the evaporation mechanism comprises an evaporator, a stirring assembly for accelerating liquid evaporation is arranged on the evaporator, a first condenser is connected to a discharge port of the evaporator, a separation mechanism for separating BDO residual liquid is connected to a discharge port of the first condenser, and an oxidation reaction mechanism is connected to a discharge port of the separation mechanism;
the evaporator comprises an evaporation tank body, the stirring assembly is arranged on the evaporation tank body, the stirring assembly comprises a motor bracket arranged on the evaporation tank body, the middle part of the motor bracket is connected with a motor, the bottom of the motor is connected with a rotating shaft, and the upper part of the rotating shaft is connected with a first liquid distributor; the lower part of the rotating shaft is connected with a connecting plate, scraping plates are arranged at two ends of the connecting plate, a stirring rod is connected inside the scraping plates, and one end, away from the scraping plates, of the stirring rod is welded with the rotating shaft;
the top of the evaporation tank body is provided with a feed inlet and an exhaust outlet respectively at two sides of the motor bracket; the right side of the bottom of the evaporation tank body is connected with a circulating pump, the top of the circulating pump is connected with a guide pipe, and a discharge hole of the guide pipe is communicated with the first liquid distributor;
the evaporator comprises a first evaporator and a second evaporator, wherein a discharge port of the first evaporator is connected with a material pumping pump, and a discharge port of the material pumping pump is communicated with a feed inlet of the second evaporator; the exhaust port of the second evaporator is communicated with the first condenser, the exhaust port of the first evaporator is connected with the second condenser, and the second condenser is communicated with the combustion mechanism;
the separation mechanism comprises a layered cavity, a drainage control assembly is arranged at the bottom of the layered cavity, the output end of the drainage control assembly is connected with a drainage tube, the discharge port of the drainage tube is connected with the oxidation reaction mechanism, a siphon is arranged on the layered cavity, and the other end of the siphon is communicated with the second evaporator;
the oxidation reaction mechanism comprises an oscillation generator, the output end of the oscillation generator is connected with a feeding section, the discharge port of the feeding section is connected with a reactor main body, the reactor main body comprises a reaction tank body, a liquid distribution plate is arranged in the reaction tank body, a plurality of uniformly distributed water cap holes are formed in the liquid distribution plate, and water caps are detachably connected to the water cap holes;
a rectifying mechanism is arranged on a discharge hole of the reactor main body;
the combustion mechanism comprises a combustion boiler which is respectively connected with the evaporation mechanism and the rectification mechanism and is used for receiving the tailings of the evaporation mechanism and the rectification mechanism and burning the tailings to provide heat for the evaporation mechanism and the rectification mechanism.
2. A separation device for purifying BDO from BDO waste liquid according to claim 1, wherein: the first condenser and/or the second condenser comprises a condensing chamber I, a condensing pipe I is arranged in the condensing chamber I, and the condensing pipe I is in a spiral structure.
3. A separation device for purifying BDO from BDO waste liquid according to claim 1, wherein: the liquid distribution plate comprises a first distribution plate, a second distribution plate and a third distribution plate which are arranged in the tank body from top to bottom in sequence, the diameter of the second distribution plate is larger than that of the first distribution plate or the third distribution plate, and the diameters of the first distribution plate and the third distribution plate are equal; and a packing layer is arranged among the first distribution plate, the second distribution plate and the third distribution plate, and random packing made of ceramic materials or glass materials is filled in the packing layer.
4. A separation device for purifying BDO from BDO waste liquid according to claim 3, wherein: the top and the bottom of the reaction tank body are respectively provided with a first end cover and a second end cover, the first end cover is provided with a discharge hole, the second end cover is provided with a feed inlet matched with the feed section, and the feed inlet is provided with a second liquid distributor.
5. A separation device for purifying BDO from BDO waste liquid according to claim 1, wherein: the rectification mechanism comprises a rectification tower, a third condensation mechanism is arranged at the bottom of the rectification tower and comprises a condensation chamber II, a condensation pipe II is arranged in the condensation chamber II, and the other end of the condensation pipe II extends to the outer side of the right lower end of the condensation chamber II; the rectifying tower is characterized in that a tower plate assembly is arranged inside the rectifying tower and is formed by sequentially and alternately arranging annular tower plates and circular tower plates up and down, the annular tower plates and the circular tower plates are horizontally arranged, the annular tower plates are arranged on the tower wall of the rectifying tower, and the circular tower plates are connected with the tower wall of the rectifying tower through connecting rods.
6. A separation device for purifying BDO from BDO waste liquid according to claim 5, wherein: the rectifying tower comprises a first rectifying tower and a second rectifying tower, a condensing chamber III is connected to an exhaust port of the first rectifying tower, a condensing pipe III is installed in the condensing chamber III, and the other end of the condensing pipe III is communicated with a feed inlet of the combustion mechanism; the condenser pipe II that first rectifying column bottom was established with the feed inlet of second rectifying column is linked together, be connected with condensation chamber IV on the gas vent of second rectifying column, install condensation pipe IV in the condensation chamber IV, condensation chamber IV's lower extreme fixedly connected with row material pipe, condensation pipe IV's lower extreme with arrange the upper end of material pipe and put through each other, connect the material bottle is installed to row material pipe's tip.
CN202311343328.9A 2023-10-17 2023-10-17 Separation device for purifying BDO from BDO waste liquid Active CN117065379B (en)

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JP2021116246A (en) * 2020-01-23 2021-08-10 リファインホールディングス株式会社 Purified 1,3-butanediol and its manufacturing method
CN114669073A (en) * 2022-04-01 2022-06-28 南京菲特工业科技有限公司 1,4-butanediol multi-effect rectification device system and multi-effect rectification process
CN115779472A (en) * 2022-12-29 2023-03-14 云南唯益新材料有限公司 Refining method and rectifying device for crude butanol in 1, 4-butanediol production
CN116808610A (en) * 2023-08-31 2023-09-29 福建聚创新材料科技有限公司 Scraper type film scraping evaporation device for treating BDO residual liquid

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CN202214307U (en) * 2011-09-21 2012-05-09 新疆美克化工股份有限公司 1,4-butanediol residual liquid recycling system
JP2021116246A (en) * 2020-01-23 2021-08-10 リファインホールディングス株式会社 Purified 1,3-butanediol and its manufacturing method
CN114669073A (en) * 2022-04-01 2022-06-28 南京菲特工业科技有限公司 1,4-butanediol multi-effect rectification device system and multi-effect rectification process
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