Device for removing chloride ions and formaldehyde in amino trimethylene phosphonic acid
By designing a device including a reactor, an absorption tank and a vacuum pump, the combination of evaporator and condenser is used to solve the problems of high steam consumption and low production efficiency in the removal process of chloride ions and formaldehyde in the prior art, and a more efficient and environmentally friendly production process is achieved.
Patent Information
- Application Number
- CN202510665478.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-22
- Publication Date
- 2025-06-27
AI Technical Summary
When the prior art reduces the chloride ions and formaldehyde content in aminotrimethylene phosphoric acid (ATMP), steam consumption is high, production efficiency is low, production cost is high, and wastewater treatment volume and electricity energy are increased, resulting in an increase in treatment cost and carbon emissions.
A device including a reactor, an absorption tank and a vacuum pump is designed. Through the combination of an evaporator and a condenser, the effect of a falling film evaporator and a vacuum pump is achieved to achieve effective removal of chloride ions and formaldehyde.
The device reduces steam usage, improves production efficiency, reduces production costs, and reduces wastewater treatment and electricity consumption, reducing treatment costs and carbon emissions.
Smart Images
Figure CN120205073A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a device for removing chloride ions and formaldehyde from water treatment agents. Specifically, it is a device for removing chloride ions and formaldehyde from aminotrimethylenephosphonic acid. Background Art
[0002] In the field of chemical production, it is known that the water treatment agent aminotrimethylenephosphonic acid (ATMP) is formed by putting chemical raw materials such as ammonium chloride, phosphorous acid and formaldehyde into a reaction kettle for reaction. After the reaction, the content of chloride in aminotrimethylenephosphonic acid (ATMP) is 5 - 6%, and the content of formaldehyde is 3 - 5%. However, the chloride content required for the finished product quality is less than 1%. For many foreign trade orders, the requirement for chloride content is even less than or equal to 0.5%. Thus, it can be seen that the chloride content of 5 - 6% in the aminotrimethylenephosphonic acid (ATMP) after reaction is far higher than the chloride content of less than 1% required for the finished product quality. Therefore, it is necessary to further reduce the chloride content to meet the requirement of less than 1%.
[0003] Currently, the method for reducing the chloride content in aminotrimethylenephosphonic acid (ATMP) is as follows: after the reaction is completed, steam is directly introduced into the reaction kettle to heat the aminotrimethylenephosphonic acid (ATMP) to 100 - 140 °C. By raising the temperature and supplemented with vacuum pumping, the chloride ions and formaldehyde in the aminotrimethylenephosphonic acid (ATMP) are directly discharged from the reaction kettle together with the gas. Although this method can remove the chloride ions and formaldehyde in the aminotrimethylenephosphonic acid (ATMP) to meet the requirement of less than 1%. However, to meet the requirement of chloride ions less than or equal to 1%, taking a reaction kettle with a capacity of 5000 liters as an example, it is necessary to introduce steam into the reaction kettle for 8 - 10 hours, resulting in a large amount of steam consumption, low production efficiency and high production cost. Also, due to the increase in temperature, the water, chloride ions and formaldehyde in the aminotrimethylenephosphonic acid (ATMP) are directly discharged from the reaction kettle together with the gas. The water in the gas is not condensed into water for collection and reuse, resulting in a large amount of wastewater generated. In this way, not only the amount of wastewater treatment and electric energy are increased, but also the production cost and carbon emission are increased. Summary of the Invention
[0004] The problem to be solved by the present invention is to provide a device for removing chloride ions and formaldehyde from aminotrimethylenephosphonic acid. By using this device, not only can the steam consumption be reduced, the production efficiency be improved and the production cost be lowered. Moreover, the amount of wastewater treatment and electric energy can be reduced, and the treatment cost and carbon emission can be lowered.
[0005] The above problems to be solved by the present invention are achieved by the following technical solutions: The device for removing chloride ions and formaldehyde from amino trimethylene phosphonic acid according to the present invention comprises a reaction kettle, an absorption tank and a vacuum pump. The top of the reaction kettle is provided with a first feed inlet, a stirrer and a return port, and the bottom thereof is provided with a first discharge outlet. The top of the absorption tank is provided with a second air inlet and a third air outlet. The third air outlet is communicated with the inlet of the vacuum pump through a pipeline. Its characteristics are as follows: an evaporator and a condenser are arranged between the reaction kettle and the absorption tank. The top of the evaporator is provided with a second feed inlet, a first air outlet and a spraying mechanism, and the bottom thereof is provided with a second discharge outlet. Steam inlets and liquid inlets are respectively arranged on the side walls on both sides of the second discharge outlet. The bottom of the condenser is provided with a liquid outlet and a second air outlet, the top thereof is provided with a first air inlet, and condensate inlets and condensate outlets are respectively arranged on the opposite sides of the lower part and the upper part thereof. The first discharge outlet is communicated with the second feed inlet through a first transfer pump and a pipeline, the first air outlet is communicated with the first air inlet through a pipeline, and the second air outlet is communicated with the second air inlet through a pipeline. The liquid outlet is communicated with the liquid inlet through a pipeline, the second discharge outlet is communicated with the return port through a pipeline, and the steam inlet is communicated with a steam source.
[0006] Wherein, the evaporator is a falling film evaporator, which comprises a cylindrical outer shell, the cylindrical outer shell is a jacketed outer shell, and a columnar graphite block is arranged therein. Vertical through holes are uniformly distributed on the columnar graphite block. The steam inlet is communicated with the jacket inner cavity of the jacketed outer shell.
[0007] A further improvement scheme of the present invention is that the outlet of the vacuum pump is communicated with the second air inlet of the absorption tank through a second transfer pump and a pipeline.
[0008] A further improvement scheme of the present invention is that a water discharge port is arranged on one side of the bottom of the absorption tank.
[0009] A further improvement scheme of the present invention is that a temperature measuring port is arranged on the top of the evaporator, and a thermometer is arranged in the temperature measuring port.
[0010] A further improvement scheme of the present invention is that a sampling port and a valve are arranged on the pipeline between the second discharge outlet and the return port.
[0011] The vacuum pump is any one of a water jet vacuum pump, a valve plate vacuum pump, a screw vacuum pump and a water circulation vacuum pump.
[0012] A further improvement scheme of the present invention is that the vacuum pump is a corrosion-resistant vacuum pump.
[0013] Since there are an evaporator and a condenser between the reaction kettle and the absorption tank. The top of the evaporator has a second feed inlet, a first gas outlet and a spraying mechanism, and its bottom has a second discharge outlet. On the side walls on both sides of the second discharge outlet, there are a steam inlet and a liquid inlet respectively. The bottom of the condenser has a liquid outlet and a second gas outlet, its top has a first gas inlet, and on the opposite sides of its lower and upper parts, there are a condensate inlet and a condensate outlet respectively. The first discharge outlet is communicated with the second feed inlet by means of a first transfer pump and a pipeline, the first gas outlet is communicated with the first gas inlet by means of a pipeline, and the second gas outlet is communicated with the second gas inlet through a pipeline. The liquid outlet is communicated with the liquid inlet by means of a pipeline, the second discharge outlet is communicated with the said return port by means of a pipeline, and the steam inlet is communicated with a steam source. During operation, while passing steam to the lower part of the evaporator and spraying ionized water into the evaporator by the spraying mechanism, the amino trimethylene phosphonic acid (ATMP) after being reacted in the reaction kettle is sent into the upper part of the evaporator through the first transfer pump, pipeline and the second feed inlet. After the amino trimethylene phosphonic acid (ATMP) entering the evaporator is evaporated, the water, chloride ions and formaldehyde in it are sent into the condenser together with the steam from the top of the evaporator through the pipeline and the first gas inlet, and the evaporated and treated amino trimethylene phosphonic acid (ATMP) flows back into the reaction kettle through the second discharge outlet and the pipeline. The gas entering the condenser is condensed into a liquid and then sent into the bottom of the evaporator through the liquid outlet, pipeline and liquid inlet, and flows back into the reaction kettle together with the evaporated and treated amino trimethylene phosphonic acid (ATMP). The chloride ions and formaldehyde entering the condenser are absorbed into the absorption tank under the action of a vacuum pump. Thus, a large amount of chloride ions and formaldehyde in the amino trimethylene phosphonic acid are removed.
[0014] Since in the present invention, a steam inlet is arranged on the side wall of the lower part of the evaporator, during the working process, the evaporator is directly heated by passing steam. Through multiple tests, taking a reaction kettle with a capacity of 5000 liters as an example, it only takes about 4 hours to reduce the chloride ions in the amino trimethylene phosphonic acid (ATMP) to less than 1%. Compared with the background technology that it takes 8 - 10 hours to pass steam to heat the reaction kettle to reduce the chloride ions in the amino trimethylene phosphonic acid (ATMP) to less than 1%, not only the steam consumption is reduced, the production efficiency is improved, and the production cost is reduced. Moreover, the amount of wastewater treatment and electric energy are reduced, and the treatment cost and carbon emission are reduced. Brief Description of the Drawings
[0015] Figure 1 It is a schematic structural diagram of the device for removing chloride ions and formaldehyde in amino trimethylene phosphonic acid of the present invention. Detailed Embodiments
[0016] As Figure 1 shown, the device for removing chloride ions and formaldehyde in amino trimethylene phosphonic acid of the present invention comprises a reaction kettle 1, an evaporator 2, a condenser 3, an absorption tank 4 and a vacuum pump 5.
[0017] A first feed inlet 11, a stirrer 12, and a return port 13 are provided at the top of the reactor 1, and a first discharge port 15 is provided at the bottom thereof.
[0018] The evaporator 2 is a falling film evaporator, which includes a cylindrical outer shell. The cylindrical outer shell is a jacketed outer shell, and a columnar graphite block 28 is installed therein. Vertical through holes are evenly distributed on the columnar graphite block 28. The number of the columnar graphite blocks 28 can be determined according to needs, and can be one section, two sections or more than two sections. In this embodiment, the columnar graphite block 28 is three sections, and the three-section columnar graphite blocks 28 are stacked vertically along the inner cavity of the cylindrical outer shell, and their vertical through hole numbers are the same and correspond to each other one by one. A second feed inlet 21, a first gas outlet 23, and a spraying mechanism 22 are provided at the top of the evaporator 2, and a second discharge port 26 is provided at the bottom thereof. Steam inlets 27 and liquid inlets 25 are respectively machined on the side walls on both sides of the second discharge port 26, and both the steam inlet 27 and the liquid inlet 25 are located on the opposite sides at the bottom of the cylindrical outer shell. Among them, a steam outlet 271 is machined on the upper part of the cylindrical outer shell on the opposite side of the steam inlet 27, and the steam outlet 271 is connected to a water conveying valve through a pipeline.
[0019] The outer shell of the condenser 3 is jacketed. A liquid outlet 34 and a second gas outlet 32 are machined at the bottom thereof, and a first gas inlet 31 is machined at the top thereof. The liquid outlet 34, the second gas outlet 32, and the first gas inlet 31 are all communicated with the inner cavity of the condenser 3. A condensate inlet 33 and a condensate outlet 35 on the opposite side walls of the lower part and the upper part of the condenser 3 are both communicated with the inner cavity of its jacketed outer shell. A refrigerator for cooling the refrigerant is connected between the condensate inlet 33 and the condensate outlet 35.
[0020] A second gas inlet 41 and a third gas outlet 42 are machined at the top of the absorption tank 4, and a water discharge port 43 is machined on one side at the bottom thereof. The third gas outlet 42 is communicated with the inlet 51 of the vacuum pump 5 through a pipeline.
[0021] The first discharge port 15 of the reactor 1 is communicated with the second feed inlet 21 on the evaporator 2 through a first transfer pump 16 and a pipeline. The first gas outlet 23 of the evaporator 2 is communicated with the first gas inlet 31 at the top of the condenser 3 through a pipeline. The second gas outlet 32 at the bottom of the condenser 3 is communicated with the second gas inlet 41 on the absorption tank 4 through a pipeline. The third gas outlet 42 of the absorption tank 4 is communicated with the inlet of the vacuum pump 5 through a pipeline, and the outlet of the vacuum pump 5 is connected to the second gas inlet 41 at the top of the absorption tank 4 through a second transfer pump 7 and a pipeline. The liquid outlet 34 of the condenser 3 is communicated with the liquid inlet 25 of the evaporator 2 through a pipeline. The second discharge port 26 of the evaporator 2 is communicated with the return port 13 of the reactor 1 through a pipeline. The steam inlet 27 of the evaporator 2 is respectively connected to the outlet of a steam source (boiler) and the jacket inner cavity of the jacketed outer shell through a pipeline.
[0022] The absorption tank 4 can be one, or multiple ones can be provided as needed. The specific quantity can be determined according to requirements. If there are two absorption tanks 4, the third air outlet 42 of the previous absorption tank 4 is communicated with the second air inlet 41 of the subsequent absorption tank 4. The second air inlet 41 of the previous absorption tank 4 is communicated with the second air outlet 32 of the condenser 3. The third air outlet 42 of the subsequent absorption tank 4 is communicated with the inlet of the vacuum pump 5 through a pipeline. The drain outlet 52 of the vacuum pump 5 is communicated with the second air inlet 41 of the previous absorption tank 4 by means of the second delivery pump 7.
[0023] To facilitate measuring the temperature inside the evaporator 2, a temperature measuring port is machined at the top of the evaporator 2, and a thermometer 24 is arranged inside the temperature measuring port.
[0024] To facilitate grasping the chloride ion and formaldehyde content of the material inside the bottom of the evaporator 2 at any time, a sampling port 29 is machined on the pipeline between the second discharge port 26 and the material return port 13, and a valve 291 is installed at the sampling port 29.
[0025] The vacuum pump 5 is any one of a water jet vacuum pump, a vane vacuum pump, a screw vacuum pump, and a water circulation vacuum pump. In this embodiment, the vacuum pump is a water jet vacuum pump.
[0026] The first delivery pump 16 and the second delivery pump 7 are both corrosion-resistant delivery pumps. The vacuum pump 5 is a corrosion-resistant vacuum pump. The pipeline and the valve 291 are a corrosion-resistant pipeline and a corrosion-resistant valve respectively.
[0027] During operation, while steam is introduced into the lower part of the evaporator 2, ionized water is sprayed into the evaporator 2 by the spraying mechanism 22, and cooling water is introduced into the jacketed shell of the condenser 3 through the condensate inlet 33, the amino trimethylene phosphonic acid (ATMP) after the reaction in the reaction kettle 1 is sent into the upper part of the evaporator 2 through the first delivery pump 16, the pipeline, and the second feed port 21. After the amino trimethylene phosphonic acid (ATMP) entering the evaporator 2 is evaporated, the water, chloride ions, and formaldehyde in it, under the action of the vacuum pump 5, together with the evaporation gas, are sent into the condenser 3 from the top of the evaporator 2 through the pipeline and the first air inlet 31, while the amino trimethylene phosphonic acid (ATMP) after evaporation treatment enters the bottom of the evaporator 2. The evaporation gas entering the condenser 3 is condensed into a liquid and then sent to the bottom of the evaporator 2 through the liquid outlet 34, the pipeline, and the liquid inlet 25, and flows back into the reaction kettle 1 together with the amino trimethylene phosphonic acid (ATMP) after evaporation treatment. The chloride ions and formaldehyde entering the condenser 3 are absorbed into the absorption tank 4 under the action of the vacuum pump 5, thereby removing a large amount of chloride ions and formaldehyde in the amino trimethylene phosphonic acid.
Claims
1. An apparatus for removing chloride ions and formaldehyde from amino trimethylene phosphonic acid, comprising a reaction kettle (1), an absorption tank (4) and a vacuum pump (5); the top of the reaction kettle (1) is provided with a first feed inlet (11), a stirrer (12) and a return port (13), and its bottom is provided with a first discharge outlet (15); the top of the absorption tank (4) is provided with a second air inlet (41) and a third air outlet (42); the third air outlet (42) is communicated with the inlet (51) of the vacuum pump (5) through a pipeline; it is characterized in that: There is an evaporator (2) and a condenser (3) between the reaction kettle (1) and the absorption tank (4); the top of the evaporator (2) has a second feed inlet (21), a first gas outlet (23) and a spraying mechanism (22), and its bottom has a second discharge outlet (26); on the side walls on both sides of the second discharge outlet (26), there are a steam inlet (27) and a liquid inlet (25) respectively; the bottom of the condenser (3) has a liquid outlet (34) and a second gas outlet (32), its top has a first gas inlet (31), and on the opposite sides of its lower part and upper part, there are a condensate inlet (33) and a condensate outlet (35) respectively; the first discharge outlet (15) is communicated with the second feed inlet (21) by means of a first transfer pump (16) and a pipeline, the first gas outlet (23) is communicated with the first gas inlet (31) by means of a pipeline, and the second gas outlet (32) is communicated with the second gas inlet (41) by means of a pipeline; the liquid outlet (34) is communicated with the liquid inlet (25) by means of a pipeline, the second discharge outlet (26) is communicated with the return port (13) by means of a pipeline, and the steam inlet (27) is communicated with a steam source.
2. The device for removing chloride ions and formaldehyde from amino trimethylene phosphonic acid according to claim 1, characterized in that: The evaporator (2) is a falling film evaporator, which contains a cylindrical outer shell, and the cylindrical outer shell is a jacketed outer shell, and there is a columnar graphite block (28) inside it. The columnar graphite block (28) is evenly provided with vertical through holes; the steam inlet (27) is communicated with the jacket inner cavity of the jacketed outer shell.
3. The device for removing chloride ions and formaldehyde from amino trimethylene phosphonic acid according to claim 1, wherein: The outlet of the vacuum pump (5) is communicated with the second gas inlet (41) of the absorption tank (4) by means of a second transfer pump (7) and a pipeline.
4. The device for removing chloride ions and formaldehyde from amino trimethylene phosphonic acid according to claim 1, wherein: On one side of the bottom of the absorption tank (4), there is a water discharge port (43).
5. The device for removing chloride ions and formaldehyde from amino trimethylene phosphonic acid according to claim 1, wherein: The top of the evaporator (2) has a temperature measuring port, and there is a thermometer (24) inside the temperature measuring port.
6. The device for removing chloride ions and formaldehyde from amino trimethylene phosphonic acid according to claim 1, characterized in that: On the pipeline between the second discharge outlet (26) and the return port (13), there is a sampling port (29) and a valve (291).
7. The device for removing chloride ions and formaldehyde from amino trimethylene phosphonic acid according to claim 1, characterized in that: The vacuum pump (5) is any one of a water jet vacuum pump, a valve type vacuum pump, a screw type vacuum pump and a water circulation vacuum pump.
8. The device for removing chloride ions and formaldehyde in aminotrimethylene phosphonic acid according to any one of claims 1 to 7, wherein the vacuum pump (5) is a corrosion-resistant vacuum pump.