1, 4 butynediol solution deionization device

Abstract

The utility model discloses a 1, 4-butynediol solution desorption device which is characterized in that 1, 4-butynediol and water are completely evaporated by adopting a vacuum distillation method, so that ions and other dissolved matters are attached to a reboiler tube nest of a distillation tower after being concentrated and separated out. The two distillation towers are connected in series, so that the steam consumption can be saved, and the cost is reduced. One reboiler is opened and the other reboiler is standby, and can be subjected to isolated cleaning after on-line switching, so that continuous operation of the device is realized. The outlets of the two tower bottom circulating extraction pumps are respectively provided with a filter, ions and precipitates in the concentrated 1, 4-butynediol solution are filtered, and the single-time use time of the reboiler is prolonged. According to the present invention, the physical change of the 1, 4-butynediol solution is utilized to remove the ions in the 1, 4-butynediol solution, the use of acid and alkali is not required, the high-salt and strong-corrosivity wastewater is not generated any more, the sewage treatment difficulty is reduced, and the environmental protection pressure is reduced. Meanwhile, the safety risk of operators in the working period is reduced, and the production safety of the device is improved.

Description

Technical Field

[0001] This utility model relates to the technical field of 1,4-butanediol production via the acetylacetonate process, and more particularly to a 1,4-butynediol solution deionization device. It is used to remove ions from the 1,4-butynediol solution, an intermediate product of the 1,4-butanediol production process, while simultaneously eliminating the generation of high-salt wastewater during operation in chemical and other production processes. Background Technology

[0002] Currently, the intermediate product 1,4-butynediol in the acetylacetylene-aldehyde process for producing 1,4-butanediol contains Na. + Ca2 + Mg2 + Cu + Plasma significantly impacts subsequent hydrogenation reactions and can easily poison hydrogenation catalysts. In actual production, cation and anion exchange resins are primarily used for deionization. However, resin regeneration requires the use of acids and alkalis, generating large amounts of highly saline and corrosive wastewater, increasing the difficulty of wastewater treatment and placing significant environmental pressure on the industry. During production, the temperature of the 1,4-butynediol solution is around 142℃, while the resin's operating temperature must be below 60℃. High temperatures cause resin pulverization, reduced performance, and a shortened lifespan, while cooling results in heat loss. In recent years, influenced by the international and domestic business environment and the continuous release of domestic 1,4-butanediol production capacity, businesses have faced considerable difficulties. Furthermore, the stringent environmental regulations have further exacerbated the challenges for 1,4-butanediol producers. When producing 1,4-butanediol using the acetylacetone-aldehyde method, it is necessary to remove ions from the intermediate 1,4-butynediol solution while simultaneously ensuring that no high-salt wastewater is generated during the chemical or other production processes. There is no existing device for removing ions from the intermediate product 1,4-butynediol solution. Utility Model Content

[0003] The purpose of this invention is to overcome the shortcomings of existing technologies and provide a device for deionizing 1,4-butynediol solution. This invention employs vacuum distillation to completely evaporate 1,4-butynediol and water. Ions and other dissolved substances are concentrated and precipitated, adhering to the reboiler tubes of the distillation column. The reboiler is designed with one operating and one standby unit to ensure continuous operation of the device. Furthermore, this device does not require the use of acids or alkalis during operation, eliminating the generation of high-salt and highly corrosive wastewater and reducing the difficulty of wastewater treatment. Due to the high temperature of the material, the increase in steam consumption during device operation is relatively low.

[0004] This utility model is achieved through the following technical solution:

[0005] A 1,4-butynediol solution deionization device includes a first section comprising a distillation column, a reboiler, a bottom circulation pump, a filter, a primary condenser, a vacuum pump, a condensate collection tank, and a top pump. The outlet of the reboiler is connected to the inlet of the distillation column, the top outlet of the distillation column is connected to the inlet of the primary condenser, the outlet of the primary condenser is connected to the inlet of the condensate collection tank, the vacuum pump is connected to the vent line of the primary condenser, and the outlet of the condensate collection tank is connected to the inlet of the top pump. The bottom outlet of the distillation column is connected to the inlet of the bottom circulation pump, the outlet of the bottom circulation pump is connected to the inlet of the filter, and the outlet of the filter is connected to the inlet of the reboiler.

[0006] The reboiler is provided in two units, which are connected in parallel.

[0007] It also includes a secondary condenser, which is connected in series with the primary condenser, and the vent line of the secondary condenser is connected to a vacuum pump.

[0008] The vacuum pump mentioned is either a steam jet vacuum pump or a liquid ring centrifugal vacuum pump.

[0009] The filter consists of two filters connected in parallel, and the filters use filter bags with a precision of 1μm or higher.

[0010] It also includes a second-stage unit identical to the first-stage unit, with the outlet of the filter in the first-stage unit connected in series with the distillation column of the second-stage unit.

[0011] This invention utilizes two identical sets of devices connected in series to enhance the ability to remove ions from the material. The distillation columns are designed in series to improve evaporation efficiency while saving steam consumption. Two reboilers are used per distillation column, one operating and one on standby. After evaporation, precipitates adhere to the tube walls of the reboilers, affecting heat exchange and reducing load. Regular switching and cleaning can be performed to ensure the device's operating load. Two bottom circulation pumps are designed for each distillation column to ensure continuous operation. Their main function is to circulate and transport the material at the bottom of the distillation columns. Four bag filters are designed to operate in parallel, using filter bags with a precision of less than 1μm to filter precipitates from the concentrated material, effectively separating them. One primary condenser is designed for each distillation column, condensing the gaseous material into a liquid phase via circulating water. The liquid enters a condensate collection tank and is then pumped to a storage tank via a top pump. Each distillation column is equipped with one secondary condenser, primarily supplementing the primary condenser. It also uses circulating water to condense the gaseous material from the distillation column into a liquid phase, which then enters the condensate collection tank. The primary and secondary condensers, along with the vacuum pump, work together to reduce the pressure within the distillation column, maintaining a high vacuum condition, lowering the evaporation temperature of the material, saving steam consumption, and stabilizing the physical properties of 1,4-butynediol. The column top pump transports the deionized material condensed from the primary and secondary condensers to the intermediate tank area; one pump is operational while another is on standby. The piping control system connects the relevant equipment via pipes and valves to ensure the normal operation of the unit.

[0012] The distillation column, reboiler, bottom circulation pump, filter, primary condenser, secondary condenser, vacuum pump, condensate collection tank, and top pump consist of two sets of equipment connected in series to improve the ability to remove ions from the material.

[0013] The distillation column operates under high vacuum, which reduces the evaporation temperature of the material, saves steam consumption, and stabilizes the physical properties of 1,4-butynediol.

[0014] The reboilers used in the two stages differ in their heat sources. The first-stage distillation column reboiler uses the bottom feed from the 1,4-butanediol stripping column of the original production unit. This feed has a temperature of approximately 142°C. After passing through the reboiler, the feed enters the distillation column, where the water and a small portion of the 1,4-butanediol are heated into a gaseous state and flow out from the top of the column. The second-stage distillation column reboiler uses 0.8 MPa steam to ensure that the feed entering the second-stage distillation column is heated and evaporated, flowing out from the top of the column. After the 1,4-butynediol solution is heated and concentrated, the precipitates will adhere to the tube walls of the reboiler, affecting the heat exchange efficiency and leading to a reduction in load. Therefore, it is necessary to periodically disconnect and clean the reboiler.

[0015] The filter is installed at the outlet of the circulating pump at the bottom of the tower, with one filter on and one on standby. When the pressure difference exceeds a certain value, the filter bag can be switched and replaced. Using filter bags with a precision of 1μm or higher, the concentrated precipitates of the material can be effectively filtered and separated.

[0016] The primary and secondary condensers are connected in series and use circulating water for cooling.

[0017] Vacuum pumps are installed in the vent lines of the primary and secondary condensers. They can be either steam jet type or liquid ring centrifugal type. As long as the non-condensable gases inside are extracted in time, the evaporator can maintain a high vacuum, thereby reducing heat consumption and stabilizing the physical properties of the material.

[0018] The condensate collection tank recovers the liquid material condensed by the primary and secondary condensers, and then sends it to the storage tank via the top pump. The top pump is also equipped with a backup pump to ensure continuous operation of the unit. The material has undergone evaporation and condensation processes, which removes the contained ions, resulting in the finished product of the unit.

[0019] The aforementioned top-of-column pumps, two of which are designed for each distillation column, are used to ensure continuous operation of the unit and to deliver the material in the condensate collection tank to the storage tank.

[0020] The piping in this device is made of stainless steel, and related equipment is connected through pipes and valves. The operating load of the device can be controlled through the valves. Pressure gauges, thermometers, level gauges, and other detection instruments are installed, enabling automatic or manual control.

[0021] This invention employs a two-stage distillation column connected in series. Utilizing the heat of the material itself, water and a small amount of 1,4-butynediol are evaporated in the first distillation column, saving steam consumption. The second distillation column uses 0.8 MPa steam as a heat source to evaporate the remaining material. After condensation by a primary condenser and a secondary condenser at the top of the column, the deionized material is obtained.

[0022] This device uses the principle of evaporation under high vacuum to change a 1,4-butynediol solution from liquid to gas, and then condenses the gas back into liquid, thereby removing ions from the material. Because the initial temperature of the raw material is relatively high, the amount of steam consumed is relatively small.

[0023] The 1,4-butynediol solution produced in the production unit first passes through a reboiler and then enters the distillation column. Under high vacuum, water and a small amount of 1,4-butynediol evaporate into a gaseous state. After condensation in the condenser at the top of the column, it undergoes a phase change and becomes liquid, entering the condensate collection tank. The condensate is then pumped from the top of the column to the tank area. A vacuum pump removes non-condensable gases to ensure high vacuum. The bottom material is recycled from the bottom of the column, pumped to a filter, and then partially enters the reboiler for heating before entering the distillation column. The remaining material enters the next distillation column. The reboiler in this distillation column uses 0.8 MPa steam, which can completely evaporate the 1,4-butynediol in the material. After condensation in the condenser at the top of the column, it undergoes a phase change and becomes liquid, entering the condensate collection tank. The condensate is then pumped from the top of the column to the tank area. A vacuum pump removes non-condensable gases to ensure high vacuum. The bottom material is recycled from the bottom of the column, pumped to a filter, heated in the reboiler, and then enters the distillation column. Through distillation in a two-stage distillation column, all ions in the material at the top of the column have been removed, which can meet the requirements of subsequent hydrogenation reaction, and at the same time, no more high-salt and highly corrosive wastewater is generated.

[0024] The advantages of this invention are as follows: This invention mainly comprises a distillation column, a reboiler, a bottom circulating pump, a filter, a primary condenser, a secondary condenser, a vacuum pump, a condensate collection tank, a top pump, and a pipeline control system. The equipment consists of two sets connected in series, simultaneously enhancing the ability to remove ions from the material. Utilizing the relatively high initial temperature of the material, the first evaporation can be completed, reducing steam consumption. The second evaporation uses 0.8 MPa steam, which can completely evaporate the 1,4-butynediol in the material. Both distillation columns operate in a high-vacuum environment, which lowers the evaporation temperature of the material, thereby reducing heat consumption. Through a simple material handling process, the deionized material is obtained at the top of the column. No acids or alkalis are needed during operation, eliminating the generation of high-salt and highly corrosive wastewater and reducing environmental pressure. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the structure of this utility model. Detailed Implementation

[0026] like Figure 1As shown, a 1,4-butynediol solution deionization device is used. The 1,4-butynediol solution is an intermediate product in the production of 1,4-butanediol via the acetylacetylene process. The device includes a distillation column 1, a reboiler 2, a bottom circulation pump 3, a filter 4, a primary condenser 5, a secondary condenser 6, a vacuum pump 7, a condensate collection tank 8, a top pump 9, and a pipeline control system. Two sets of the equipment are connected in series to enhance the ability to remove ions from the material. The 1,4-butynediol solution produced in the production unit first passes through the reboiler 2 and then enters the distillation column 1. Under high vacuum, water and a small amount of 1,4-butynediol evaporate into a gaseous state. After condensation in the top condenser, the gas undergoes a phase change and enters the condensate collection tank 8, which is then pumped to the tank area by the top pump 9. The vacuum pump 7 extracts non-condensable gases to ensure high vacuum. The bottom material is pumped from the bottom circulation pump 3 to the filter 4 for filtration. Part of the filtered material enters the reboiler 2 for heating and then enters the distillation column 1, while the remaining material enters the second stage of the distillation column. The reboiler 2 of this distillation column uses 0.8 MPa steam to completely evaporate the 1,4-butynediol in the material. After condensation in the condenser at the top of the column, the liquid undergoes a phase change and enters the condensate collection tank 8. From there, it is pumped to the tank area by the pump 9 at the top of the column. The vacuum pump 7 removes non-condensable gases to ensure a high vacuum. The bottom material is pumped to the filter 4 by the bottom circulation pump 3, filtered, and then heated in the reboiler 3 before entering the distillation column again. Through the two-stage distillation of the column 1, all ions in the material at the top of the column have been removed, meeting the requirements of the subsequent hydrogenation reaction, while eliminating the generation of high-salt and highly corrosive wastewater.

[0027] The distillation column 1 is designed in series. The feed is first heated by the reboiler 2 to improve the evaporation effect, and the material in the bottom of the column then enters the distillation column to save steam consumption.

[0028] The reboilers 2 are provided in pairs for each distillation column, with one in operation and one on standby. After the material evaporates, the precipitates will adhere to the tube walls of the reboilers 2, affecting the heat exchange efficiency and causing a decrease in load. They can be switched periodically for cleaning to ensure the operating load of the unit.

[0029] This invention is applicable to the removal of ions from the solution of 1,4-butynediol, an intermediate product of 1,4-butanediol produced by the acetylacetylene-aldehyde process. In order to reduce energy consumption, the initial temperature of the material is relatively high, and there is unused steam in the production equipment.

[0030] Based on the actual production equipment, steam is relatively easy to obtain, and can even be produced at a very low cost. The operating costs are low, and it does not produce high-salt and highly corrosive wastewater during operation, which reduces the difficulty of wastewater treatment and is beneficial to the development of enterprises.

[0031] Two pumps (one operational and one standby) are designed to collect the bottom product from distillation column 1, ensuring continuous operation of the unit. Their main function is to feed a portion of the material from the bottom of distillation column 1 into reboiler 2 and the remaining portion back into distillation column 1. Valves and drain lines are installed on the inlet and outlet pipes of the pumps to facilitate pump isolation and maintenance.

[0032] The filter 4 is installed at the outlet of the circulating pump 3 at the bottom of the tower, with one in operation and one on standby. It uses filter bags with a precision of 1μm or higher, which can effectively filter and separate the precipitates after the material is concentrated, thus extending the service life of the reboiler 2.

[0033] The first-stage condenser 5 is designed to be installed on the top outlet pipe of the distillation column 1. It condenses the gaseous material of the distillation column into liquid phase through circulating water, which enters the condensate collection tank 8 and is then sent out through the pipeline by the top pump 9.

[0034] The secondary condenser 6 is designed to be installed after the primary condenser 5. It mainly supplements the primary condenser 5. It also uses circulating water to condense the gaseous material of the distillation column into liquid phase, which enters the condensate collection tank 8.

[0035] Vacuum pump 7 can extract non-condensable gases from distillation column 1 in a timely manner to ensure a high vacuum in the distillation column, thereby reducing heat consumption and stabilizing the physical properties of the material.

[0036] Condensate collection tank 8 is designed to collect the material condensed by distillation column 2, primary condenser 5, and secondary condenser 6. This material has undergone evaporation and condensation processes, and the ions contained in it can be removed, making it the finished product of the device.

[0037] Two pumps (one operational and one standby) are designed for the top of the tower to ensure continuous operation of the unit. Their function is to pump the material from the condensate collection tank 8 out through pipelines. Valves and drains are also installed on the inlet and outlet pipelines of the pumps to facilitate pump isolation and maintenance.

[0038] This utility model's pipeline control system is made of stainless steel and connects related equipment through pipes and valves. The operating load of the device can be controlled through the valves. It is equipped with pressure gauges, thermometers, level gauges, and other detection instruments, enabling automatic or manual control.

[0039] This invention relates to a deionization device for the 1,4-butynediol solution produced by the acetylacetylene-aldehyde process. This device solves the problem of generating high-salt and highly corrosive wastewater during the deionization of the 1,4-butynediol solution, reducing production costs and increasing the use of a small amount of steam. However, the ease of obtaining steam is beneficial to the company's development.

[0040] This invention employs a series connection method to simultaneously enhance the ability to remove ions from the material. The 1,4-butynediol solution generated in the production unit first passes through a reboiler and then enters the distillation column. Under high vacuum, water and a small amount of 1,4-butynediol evaporate into a gaseous state. After condensation in the condenser at the top of the column, a phase change occurs, and the liquid enters the condensate collection tank. The liquid is then pumped from the top of the column to the tank area. A vacuum pump removes non-condensable gases to ensure high vacuum. The bottom material is circulated from the bottom of the column, pumped to a filter, and then partially enters the reboiler for heating before entering the distillation column. The remaining material enters the next distillation column. The reboiler in this distillation column uses 0.8 MPa steam, which can completely evaporate the 1,4-butynediol in the material. After condensation in the condenser at the top of the column, a phase change occurs, and the liquid enters the condensate collection tank. The liquid is then pumped from the top of the column to the tank area. A vacuum pump removes non-condensable gases to ensure high vacuum. The bottom material is circulated from the bottom of the column, pumped to a filter, and then heated in the reboiler before entering the distillation column. Through two-stage distillation, all ions are removed from the material at the top of the columns, meeting the requirements for subsequent hydrogenation reactions. Simultaneously, it eliminates the generation of high-salt and highly corrosive wastewater. Furthermore, it features a compact structure, small footprint, simple installation, low cost, and easy maintenance.

[0041] Regarding the deionization device for producing 1,4-butynediol intermediate 1,4-butynediol using the acetylacetyl method, it has the characteristic of high energy consumption, but its overall performance is outstanding when considering the high initial temperature of the material and its effective utilization, as well as the subsequent wastewater treatment.

[0042] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and not to limit it. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this utility model.

Claims

1. A 1,4-butynediol solution deionization device, characterized in that: The device includes a distillation column, a reboiler, a bottom circulation pump, a filter, a primary condenser, a vacuum pump, a condensate collection tank, and a top pump. The outlet of the reboiler is connected to the inlet of the distillation column, the top outlet of the distillation column is connected to the inlet of the primary condenser, the outlet of the primary condenser is connected to the inlet of the condensate collection tank, the vacuum pump is connected to the vent line of the primary condenser, and the outlet of the condensate collection tank is connected to the inlet of the top pump. The bottom outlet of the distillation column is connected to the inlet of the bottom circulation pump, the outlet of the bottom circulation pump is connected to the inlet of the filter, and the outlet of the filter is connected to the inlet of the reboiler.

2. The 1,4-butynediol solution deionization device according to claim 1, characterized in that: The reboiler is provided in two units, which are connected in parallel.

3. The 1,4-butynediol solution deionization device according to claim 1, characterized in that: It also includes a secondary condenser, which is connected in series with the primary condenser, and the vent line of the secondary condenser is connected to a vacuum pump.

4. The 1,4-butynediol solution deionization device according to claim 1, characterized in that: The vacuum pump mentioned is either a steam jet vacuum pump or a liquid ring centrifugal vacuum pump.

5. A 1,4-butynediol solution deionization device according to claim 1, characterized in that: The filter consists of two filters connected in parallel, and the filters use filter bags with a precision of 1μm or higher.

6. The 1,4-butynediol solution deionization device according to claim 1, characterized in that: It also includes a second-stage unit identical to the first-stage unit, with the filter outlet of the first-stage unit connected in series with the distillation column of the second-stage unit.

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