CN209797822U - 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester continuous hydrolysis device - Google Patents
2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester continuous hydrolysis device Download PDFInfo
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- CN209797822U CN209797822U CN201822234352.XU CN201822234352U CN209797822U CN 209797822 U CN209797822 U CN 209797822U CN 201822234352 U CN201822234352 U CN 201822234352U CN 209797822 U CN209797822 U CN 209797822U
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Abstract
The utility model relates to a novel 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester serialization hydrolysis unit specifically includes rectifying column, 1-N level hydrolysis unit (N is greater than or equal to 4), buffer tank, changes a plurality of, the valve is a plurality of and relevant pipeline of material pump. The device realizes continuous production of hydrolysis of 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester, improves the utilization rate of equipment, and greatly improves the production efficiency and the stability of product quality; is beneficial to realizing automatic control and large-scale industrial production, saves energy, reduces consumption, and is safe and environment-friendly. The specific equipment is as shown in the attached drawings.
Description
Technical Field
The utility model belongs to the chemical industry field relates to a serialization hydrolysis unit of ester, in particular to novel 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentamethyl ester serialization hydrolysis unit.
Background
the 2-phosphonic butane-1, 2, 4-tricarboxylic acid is prepared by respectively reacting maleic anhydride with alcohol to generate diester, dialkyl phosphite to generate tetraester, and alkyl acrylate to generate pentaester, and hydrolyzing, wherein the hydrolysis process has the following reaction principle:
。
in the prior art, the hydrolysis of 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentamethyl ester basically adopts batch kettle type hydrolysis, and has high energy consumption, low yield and poor product quality stability. In patent CN 104311596 a, the inventor discloses a single kettle type continuous hydrolysis process for pentaester of 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid, in the process of pentaester hydrolysis, spraying the pentaester of 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid obtained after esterification addition from a sprayer on the top of a hydrolysis device into the hydrolysis device, inputting water vapor from the bottom of the tower, after meeting the two, hydrolyzing, feeding the generated 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid into a storage tank from the bottom of the tower, gasifying the generated alcohol, condensing by a condenser, and feeding the gasified alcohol into a rectifying kettle. Steam is used as a heat source and a water source to hydrolyze the pentaester, and a byproduct alcohol-water mixed gas generated by hydrolysis is condensed by a condenser and then returns to an alcohol rectifying kettle, so that the energy consumption is reduced to a certain extent, the production efficiency is improved, but a more efficient pentaester hydrolysis process is to be researched and developed.
Disclosure of Invention
In order to further improve the production efficiency, reduce the cost and solve the problems in the prior art, the invention provides a continuous hydrolysis device for 2-phosphonobutane-1, 2, 4-tricarboxylic acid pentamethyl ester, which realizes the continuous output of 2-phosphonobutane-1, 2, 4-tricarboxylic acid products and effectively improves the energy utilization rate and the stability of the product quality.
a2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester continuous hydrolysis device specifically comprises a rectifying tower, an N-stage hydrolysis device and a buffer kettle, wherein a discharge port at the bottom of the rectifying tower is communicated with a feed port on the side wall at the upper end of a first-stage hydrolysis device;
In the N-stage hydrolysis device, a discharge port at the bottom of each stage of hydrolysis device from the 1 st stage to the N-1 st stage is communicated with a feed port at the upper end side wall of the next stage of hydrolysis device;
In the N-stage hydrolysis device, discharge ports at the tops of the 2 nd to the Nth hydrolysis devices are respectively communicated with a feed port on the side wall of the lower end of the previous hydrolysis device;
In the N-stage hydrolysis device, a discharge hole at the top of the 1 st-stage hydrolysis device is communicated with a gas inlet at the side wall of the middle part of the rectifying tower;
In the N-stage hydrolysis device, a discharge hole at the bottom of the Nth-stage hydrolysis device is communicated with a feed hole at the top of the buffer kettle; the discharge hole at the top of the buffer kettle is communicated with the feed inlet on the side wall of the lower part of the rectifying tower.
Wherein, N in the N-stage hydrolysis device is more than or equal to 4.
wherein, the N-stage hydrolysis device is internally provided with a flash port, and the flash port of each stage of hydrolysis device is communicated with the discharge port at the bottom of the hydrolysis device; the height of the overflow port of the 1 st stage hydrolysis device is 2000-3500mm, the heights of the overflow ports of the 1 st to Nth stage hydrolysis devices are sequentially increased, and the increase range is 100-800 mm.
Wherein, the N-stage hydrolysis device and the bottom of the buffer kettle are connected with a steam pipeline.
The utility model discloses a multistage reation kettle complete mixed flow device has improved 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentamethyl ester degree of hydrolysis, and prior art uses intermittent type kettle-type reaction more, and this is because 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentamethyl ester has five ester group to hydrolyze, including two phosphoester groups and three alcohol ester group. Since the hydrolysis temperatures of the respective ester groups are different, a batch reaction is carried out by gradient temperature rise. The hydrolysis reaction of each ester group is separated by the multi-stage hydrolysis device, the effect of continuous reaction is achieved, the hydrolysis degree is accurately controlled by setting different temperatures and the heights of the overflow ports, and the hydrolysis rate can reach more than 90% by using as few hydrolysis devices (N is more than or equal to 4) as possible.
the utility model discloses an actively mean lies in:
(1) the device realizes the continuous production of 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid, is easy to realize automatic control, improves the production efficiency and the equipment utilization rate, has stable product quality, and obtains alcohol with the content of more than 99.5 percent;
(2) The liquid level of each level of the pentaester hydrolysis device is in a gradient increasing trend, a certain pressure is provided for hydrolysis reaction through liquid level difference, and meanwhile, the hydrolysis temperature of each level of the hydrolysis device is in a gradient increasing trend, so that the hydrolysis rate is greatly improved;
(3) The hydrolysate alcohol-water mixed non-condensable gas of each stage of hydrolysis device reversely enters the preceding stage hydrolysis device to provide water source and heat for the preceding stage pentaester hydrolysis, so that the resource utilization rate is improved, and the energy conservation and consumption reduction are realized.
Drawings
fig. 1 is the structure diagram of the present invention, wherein: 1. the alcohol distillation tower comprises an alcohol distillation tower body 101, a distillation tower top discharge port, 102, a distillation tower bottom discharge port, 103, a distillation tower middle side wall gas inlet, 104, a distillation tower lower side wall gas inlet, 209, a pipeline, a 2.1-N stage hydrolysis device, 201, a hydrolysis device bottom discharge port, 202, a hydrolysis device top feed port, 203, a hydrolysis device bottom feed port, 205, a hydrolysis device top discharge port, 206, a hydrolysis device lower end side wall feed port, 207, a hydrolysis device series forward pipeline, 208, a hydrolysis device series reverse pipeline, 3, a buffer kettle, 301, a buffer kettle bottom feed port, 302, a buffer kettle bottom discharge port, 303, a buffer kettle top feed port, 304, a buffer kettle top discharge port, 305 and a pipeline. (1-N hydrolysis apparatus having the same structure, only the 1-stage hydrolysis apparatus will be described)
Detailed Description
the following will further describe the specific structure of the present invention by taking the hydrolysis device N-4 as an example with reference to fig. 1:
A novel 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester continuous hydrolysis device comprises an alcohol rectifying tower 1, a 1 st to 4 th-stage hydrolysis device 2, a buffer kettle 3, a plurality of material transfer pumps 4, a plurality of valves and related pipelines.
the alcohol rectifying tower 1 is a packing type rectifying tower, a tower top discharge hole 101 is formed in the tower top, a tower bottom discharge hole 102 is formed in the tower bottom, and feed inlets 103 and 104 are formed in the side walls of the middle portion and the lower portion of the tower respectively.
Wherein, 1 st to 4 th level hydrolysis unit 2 is equipped with top of the tower feed inlet 202 and discharge gate 205 respectively, and hydrolysis unit bottom is equipped with feed inlet 203 and discharge gate 201, and the tower upper end lateral wall is equipped with the feed inlet, and the tower lower extreme is equipped with lateral wall feed inlet 206.
Wherein, the bottom of the buffer kettle 3 is provided with a feed inlet 301 and a discharge outlet 302, and the top is provided with a feed inlet 303 and a discharge outlet 304.
The material outlet 102 at the bottom of the rectifying tower is connected with the material inlet on the side wall of the upper end of the 1 st stage hydrolysis device through a pipeline, and a valve and a material transfer pump are connected in series on the pipeline; the discharge port 201 at the bottom of the previous stage hydrolysis device of the 1 st to 4 th hydrolysis devices 2 and the feed port at the top side wall of the next stage hydrolysis device are sequentially connected end to end through a pipeline 207, and valves and a material transfer pump 4 are connected in series on the pipelines; the discharge port 205 at the top of the 4 th to 2 nd hydrolysis device 2 is respectively connected with the feed port 206 at the bottom side wall of the previous hydrolysis device through a pipeline 208; a discharge port 205 at the top of the 1 st stage hydrolysis device is connected with a gas inlet 103 on the bottom side wall of the rectifying tower through a pipeline 209, a discharge port 201 at the bottom of the 4 th stage hydrolysis device is respectively connected with a feed port 303 at the top of the buffer kettle 3 through a pipeline, and a discharge port 304 at the top of the buffer kettle is connected with a gas inlet 103 on the middle side wall of the rectifying tower through a pipeline 305;
Wherein, the 1 st to 4 th stage hydrolysis unit and the bottom of the buffer kettle are connected with a steam pipeline 5, valves are connected in series on each pipeline, and the steam input and the reaction temperature in each unit are controlled by the valve opening degree connected in series with each pipeline.
The discharge hole 205 at the top of the 1 st stage hydrolysis device is connected with the feed inlet 105 at the bottom side wall of the rectifying tower, so that the efficient utilization of heat and water and the airflow conveying of the mixed gas of the hydrolysis product alcohol and water to the rectifying tower are realized. Alcohol and steam from the 1-stage hydrolysis kettle and the buffer kettle (3) are separated in the rectifying tower, tower bottom liquid enters the 1 st-stage hydrolysis device from a discharge hole at the bottom of the tower for cyclic utilization, and high-purity alcohol is collected at the top of the tower.
wherein, rectifying column 1, 1 st to 4 th level hydrolysis unit 2 and heat preservation buffer tank 3 all are equipped with level gauge, temperature sensor and pressure sensor, have established interlock respectively between the level gauge that each device was established and correspond material transferring pump and valve, through PLC system control.
Wherein, the top discharge port 205 of the 4 th to 2 nd stage hydrolysis device 2 is respectively connected with the bottom side wall feed port 206 of the previous stage hydrolysis device through a pipeline 208.
Wherein, the liquid level in the 1 st to 4 th stage hydrolysis device is set to be gradually increased in a gradient range of 300-.
wherein the temperature in the 1 st to 4 th stages of hydrolysis devices is increased in a gradient manner at 2-10 ℃ along with the increase of the stages.
The working process of the device is as follows: 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentamethyl ester from the reaction kettle is injected into the primary hydrolysis device from a feed inlet 202 at a constant speed through a flow meter (not marked in the device) at the top of the tower, and is subjected to hydrolysis reaction by utilizing steam introduced from a feed inlet 203 at the bottom of the hydrolysis device, when the material liquid level in the first-stage hydrolysis device reaches a set liquid level, an interlocking device between a liquid level meter and a material transferring pump and a valve is automatically opened, incompletely hydrolyzed mixture is pumped into a second-stage hydrolysis device through a discharge port 201 at the bottom of the first-stage hydrolysis device through a pipeline 207, the incompletely hydrolyzed mixture is further hydrolyzed with steam introduced from a feed port at the bottom of the tower, the hydrolysis products are sequentially repeated to a fourth-stage hydrolysis device, the hydrolysis products are transferred into a buffer heat preservation kettle through a discharge port at the bottom of the hydrolysis device, and methanol-water mixed noncondensable gas which is not timely discharged enters an alcohol rectification tower through a discharge port 304 at the top of the heat preservation kettle and a feed port 104 at the lower side wall; alcohol-water mixed non-condensable gas generated by hydrolysis in the 4 th to 1 st-stage hydrolysis devices sequentially enters the previous-stage hydrolysis device through a discharge port 205 at the top of the hydrolysis device to recycle heat and water, enters an alcohol rectifying tower 1 through a pipeline 209 to be rectified, separated and purified when reaching the first-stage hydrolysis device, high-purity alcohol is collected from a discharge port 101 at the top of the rectifying tower, when bottom liquid of the rectifying tower reaches a set liquid level, an interlocking device between a liquid level meter connected with the rectifying tower and a material transfer pump and a valve is automatically started, and the bottom liquid is injected into the 1 st-stage hydrolysis device through a feed port at the upper end of the hydrolysis device to be repeatedly used for hydrolysis of the pentaester.
Wherein the hydrolysis temperature ranges of the 1 st to 4 th grade hydrolysis devices are 100-; the liquid levels in the 1 st to 4 th stages of hydrolysis devices are respectively controlled to be 2000mm, 2300 + 2500mm, 2700 + 3200mm and 3300 + 4000 mm; the hydrolysis degree ranges of the pentaester of the 1 st to 4 th-level hydrolysis devices are respectively 20-40%, 50-70%, 80-90% and 90-100%; the chromatographic content of the methanol separated from the top of the alcohol rectifying tower is more than 99.5 percent, the hydrolysis rate of the pentaester after four-stage hydrolysis is more than 99 percent, and a hydrolysis product 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid is transferred to a material storage device through a discharge hole 302 at the bottom of the buffer kettle after heat preservation treatment.
Claims (4)
1. A2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester continuous hydrolysis device specifically comprises a rectifying tower, an N-stage hydrolysis device and a buffer kettle, and is characterized in that: a discharge hole at the bottom of the rectifying tower is communicated with a feed inlet on the side wall of the upper end of the primary hydrolysis device;
in the N-stage hydrolysis device, a discharge port at the bottom of each stage of hydrolysis device from the 1 st stage to the N-1 st stage is communicated with a feed port at the upper end side wall of the next stage of hydrolysis device;
In the N-stage hydrolysis device, discharge ports at the tops of the 2 nd to the Nth hydrolysis devices are respectively communicated with a feed port on the side wall of the lower end of the previous hydrolysis device;
In the N-stage hydrolysis device, a discharge hole at the top of the 1 st-stage hydrolysis device is communicated with a gas inlet at the side wall of the middle part of the rectifying tower;
In the N-stage hydrolysis device, a discharge hole at the bottom of the Nth-stage hydrolysis device is communicated with a feed hole at the top of the buffer kettle; the discharge hole at the top of the buffer kettle is communicated with the feed inlet on the side wall of the lower part of the rectifying tower.
2. The apparatus of claim 1, wherein N in the N-stage hydrolysis apparatus is 4 or more.
3. The device of claim 1, wherein the N-stage hydrolysis device is provided with a flash port, and the flash port of each stage of hydrolysis device is communicated with a discharge port at the bottom of the hydrolysis device; the height of the overflow port of the 1 st stage hydrolysis device is 2000-3500mm, the heights of the overflow ports of the 1 st to Nth stage hydrolysis devices are sequentially increased, and the increase range is 100-800 mm.
4. The apparatus of claim 1, wherein the N-stage hydrolysis apparatus and the bottom of the buffer tank are connected to a steam pipeline.
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| CN201822234352.XU CN209797822U (en) | 2018-12-28 | 2018-12-28 | 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester continuous hydrolysis device |
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| CN201822234352.XU CN209797822U (en) | 2018-12-28 | 2018-12-28 | 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid pentaester continuous hydrolysis device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400644A (en) * | 2018-12-28 | 2019-03-01 | 山东泰和水处理科技股份有限公司 | A kind of 2- phosphonobutane -1,2,4- tricarboxylic acids five-ester continuous hydrolyzing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109400644A (en) * | 2018-12-28 | 2019-03-01 | 山东泰和水处理科技股份有限公司 | A kind of 2- phosphonobutane -1,2,4- tricarboxylic acids five-ester continuous hydrolyzing method |
| CN109400644B (en) * | 2018-12-28 | 2024-08-30 | 山东泰和科技股份有限公司 | Continuous hydrolysis method of 2-butane phosphonate-1, 2, 4-tricarboxylic acid five ester |
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Address after: No. 1, Shiliquan East Road, Zaozhuang City, Shandong Province, 277800 Patentee after: Shandong Taihe Technology Co.,Ltd. Address before: 277000 No.1, Shiliquan East Road, Shizhong District, Zaozhuang City, Shandong Province Patentee before: SHANDONG TAIHE WATER TREATMENT TECHNOLOGIES Co.,Ltd. |