CN210595870U - Continuous production device for organic phosphine crystals - Google Patents
Continuous production device for organic phosphine crystals Download PDFInfo
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- CN210595870U CN210595870U CN201921594694.0U CN201921594694U CN210595870U CN 210595870 U CN210595870 U CN 210595870U CN 201921594694 U CN201921594694 U CN 201921594694U CN 210595870 U CN210595870 U CN 210595870U
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Abstract
The utility model belongs to fine chemical production equipment field, concretely relates to organic phosphine crystal serialization apparatus for producing. The device comprises an organic phosphine liquid product tank, a heater, a gas-liquid separator, a distillation concentration kettle, a cooling heat exchanger, a 1-n-stage crystallization kettle, a centrifugal machine, related pipelines, valves and a material transferring pump, wherein the crystallization kettle is connected in series end to end. The utility model discloses an adopt the multistage crystallization cauldron of end to end series connection, make the material realize the natural gradient cooling when continuously shifting over to next-level crystallization cauldron in 1 to (n-1) level crystallization cauldron, need not to carry out circulative cooling, water conservation and consumption reduction, improve equipment's utilization ratio. The design of the device is beneficial to uniform mixing of materials in the crystallization kettles at all levels, crystal growth and improvement of the yield of solid products. A PLC interlocking device is built between each crystallization kettle liquid level meter or weighing unit and the feeding valve thereof, so that automatic, rapid and continuous material transfer between all levels of crystallization kettles is completed, the continuous crystallization of organic phosphonic acid products and the stable product quality are realized, and the industrialization is easy to realize.
Description
Technical Field
The utility model belongs to the technical field of fine chemicals apparatus for producing, concretely relates to serialization apparatus for producing of organic phosphine crystal.
Background
Organic phosphonic acids such as hydroxyethylidene diphosphonic acid (HEDP for short) and aminotrimethylene phosphonic acid (ATMP for short) are a cathode type corrosion inhibitor, belong to non-stoichiometric scale inhibitor, have obvious limit-dissolving effect, can form stable chelate with various metal ions such as calcium, magnesium, iron, copper, zinc and the like, can dissolve oxide on the metal surface, and have obvious synergistic interaction with other monomers, so the organic phosphonic acids are widely used as water quality stabilizers in the industrial fields of circulating cooling water, oilfield water injection, textile printing and dyeing water and the like.
Most of HEDP and ATMP conventional products supplied by the market at present are liquid products with the activity content of 50-60%, in recent years, with the continuous development of industrial requirements, the application fields of HEDP and ATMP with the characteristics of low toxicity, strong thermal stability and the like are continuously developed, and the synthetic process methods of solid hydroxyethylidene diphosphonic acid or amino trimethylene phosphonic acid solid are introduced in Chinese patents such as CN107522740A, CN101597305B and CN 1312163C. The high-purity product synthesized by the crystallization method can be used as high-end fields of catering detergents and cosmetic additives, metallurgical extracting agents, cyanide-free electroplating additives, medicines, electronics and the like, but the existing single-kettle type crystallization production device for the solid products cannot meet the increasing market demand of the like products, and the research and development of a production device and a method with higher efficiency and stable quality become one of the techniques concerned by researchers in the industry.
Disclosure of Invention
In order to solve the problems and the defects in the prior art, the invention provides a continuous production device for organic phosphine crystals.
The technical scheme of the invention is as follows:
the continuous production device for the organic phosphine crystals comprises a liquid product tank, a heater, a gas-liquid separator, a distillation concentration kettle, a 1-n-grade crystallization kettle and a centrifuge, wherein n is more than or equal to 2 and less than or equal to 8; the feed inlet of the liquid product tank is directly connected with the liquid production line, the discharge outlet of the liquid product tank is connected with the feed inlet of the heater through a pipeline, and the discharge outlet of the heater is connected with the feed inlet A of the gas-liquid separator; the distillation concentration kettle is provided with a reaction kettle jacket and a paddle type stirrer, wherein the jacket is provided with a steam inlet and a steam condensate outlet, the distillation concentration kettle is provided with a distillation concentration kettle top material inlet, a distillation concentration kettle top outlet and a distillation concentration kettle bottom material outlet, a distillation concentration kettle top feed port is connected with a gas-liquid separator bottom discharge port through a pipeline, the distillation concentration kettle top outlet is connected with a gas-liquid separator bottom feed port B, the distillation concentration kettle bottom material outlet is connected with a first-stage crystallization kettle feed port through a pipeline, each stage of crystallization kettle is provided with a top feed port and a bottom discharge port, and the next-stage crystallization kettle bottom discharge port is connected with the previous-stage top feed port; a discharge port at the bottom of the last-stage crystallization kettle is connected with a centrifugal machine; the discharge port of the centrifuge is respectively connected with the mother liquor collecting tank and the finished product tank.
Preferably, a valve and a material transferring pump are connected in series on a connecting pipeline of a discharge port of the liquid product tank and a feed port of the heater; a negative pressure pump is arranged on a connecting pipeline between an outlet at the top of the distillation concentration kettle and a feed inlet B at the bottom of the gas-liquid separator; the material outlet at the bottom of the distillation concentration kettle is connected with the connecting pipeline of the feeding port of the first-stage crystallization kettle and is connected with a material transferring pump and a cooler.
Preferably, the material of the crystallization kettle can be any one of a long and narrow reaction kettle, such as enamel, glass lining, steel lining plastic and stainless steel.
Preferably, the discharge port at the bottom of the crystallization kettle is a wide-opening hopper-shaped discharge port.
Preferably, the crystallization kettle is provided with a rod-shaped toothed stirring device, and each rod-shaped stirring tooth on the stirring device is staggered from top to bottom along the direction vertical to the stirring rod and is connected with the stirring rod in a seamless manner.
Preferably, the crystallization kettle is provided with liquid level meters or weighing units, and PLC interlocking devices in one-to-one correspondence are built between each liquid level meter or weighing unit and the corresponding feeding valve at the inlet position at the top of the crystallization kettle and the corresponding discharging valve at the discharging buckle position at the bottom of the crystallization kettle.
Preferably, a mother liquor circulating feed inlet is formed in the top of the distillation concentration kettle and connected with a mother liquor collecting tank, the mother liquor collecting tank introduces the collected mother liquor into the distillation concentration kettle for recycling the mother liquor, and the last-stage crystallization kettle is provided with a circulating water jacket layer to control the temperature in the last-stage crystallization kettle.
Preferably, the discharge port at the top of the gas-liquid separator is connected with the feed port of the cooling heat exchanger through a pipeline, and the discharge port of the cooling heat exchanger is connected with the condensate collecting tank through a pipeline.
Preferably, the device is suitable for continuous production of organic phosphine crystal products such as aminotrimethylene, hydroxyethylidene diphosphonic acid and the like.
The invention has the beneficial effects that:
(1) according to the device, the gas-liquid separator is arranged between the heater and the distillation concentration kettle, so that redundant water and low-boiling-point substances in the material can be effectively separated, the purity of the crystallized material is favorably improved, and meanwhile, the separated water and the low-boiling-point substances can be recycled for process water for synthesizing corresponding organic phosphine liquid products after being cooled and recovered;
(2) by adopting the multistage crystallization kettle devices connected in series end to end, the invention realizes natural gradient cooling while continuously transferring materials to the next-stage crystallization kettle in the 1 to (n-1) stages of crystallization kettles, does not need to carry out circulating cooling, saves water, reduces consumption and improves the utilization rate of equipment;
(3) the long and narrow crystallization kettle, the length of the stirring rod is equal to the depth of the kettle body, the rod tooth-shaped stirring device and the wide-opening hopper-shaped discharge opening device are designed, so that the uniform mixing of materials in the crystallization kettles at all levels and the crystal growth are facilitated, and the yield of solid products is improved; meanwhile, PLC automatic interlocking devices are built between the liquid level meters or weighing units arranged on the crystallization kettles and the feeding valves of the crystallization kettles, so that automatic, rapid and continuous material transfer between the crystallization kettles at different levels can be completed, the crystallization continuity of organic phosphonic acid products and the product quality can be realized, and the industrialization can be easily realized.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural diagram of each stage of crystallization kettle;
reference numerals: 1. a liquid product tank 101, a liquid product tank feed inlet 102, a liquid product tank discharge outlet, 2, a heater 201, a heater feed inlet 202, a heater discharge outlet, 3, a gas-liquid separator 301, a gas-liquid separator bottom feed inlet A, 302, a gas-liquid separator bottom discharge outlet 303, a gas-liquid separator bottom feed inlet B, 304, a gas-liquid separator gas outlet, 4, a distillation concentration kettle 401, a distillation concentration kettle top inlet 402, a distillation concentration kettle top outlet 403, a distillation concentration kettle bottom material outlet 404, an interlayer steam inlet 405, an interlayer steam condensate outlet 5, a cooler 501, a cooler feed inlet 502, a cooler discharge outlet 6, a crystallization kettle 601, a crystallization kettle feed inlet 602, a crystallization kettle discharge outlet 603, a stirring device 604, a rod-shaped stirring tooth, 605, a liquid level meter 7, a second-stage crystallization kettle, 8. the device comprises an nth-stage crystallization kettle, 9, a centrifuge, 10, a filling machine, 11, a mother liquor collecting tank, 12, a cooling heat exchanger, 13, a cooling liquid collecting tank, 14, a negative pressure pump, 15 and a pipeline a.
Detailed Description
The following is a description of the specific contents of the present invention:
the continuous production device of the organic phosphine crystal is suitable for the continuous production of organic phosphine crystal products such as aminotrimethylene, hydroxyethylidene diphosphonic acid and the like.
The device is structurally shown in figure 1 and comprises a liquid product tank 1, a heater, a gas-liquid separator, a distillation concentration kettle, a cooler 5, a 1-n-stage crystallization kettle 6 and a centrifugal machine 9, wherein n is more than or equal to 2 and less than or equal to 8.
The liquid product tank inlet 101 is directly connected with a liquid production line, the liquid product tank outlet 102 is connected with the heater inlet 201 through a pipeline, a valve and a material transferring pump are connected in series on the connecting pipeline, and the heater outlet 202 is connected with the gas-liquid separator bottom inlet A301.
The distillation concentration kettle is provided with a reaction kettle jacket and a paddle stirrer, wherein the reaction kettle jacket is provided with an interlayer steam inlet 404 and an interlayer steam condensate outlet 405, the distillation concentration kettle is provided with a distillation concentration kettle top inlet 401, a distillation concentration kettle top outlet 402 and a distillation concentration kettle bottom material outlet 403, the distillation concentration kettle top inlet 401 is connected with a gas-liquid separator bottom discharge port 302 through a pipeline, the distillation concentration kettle top outlet 402 is connected with a gas-liquid separator bottom feed inlet B303, and a negative pressure pump 14 is arranged on the connecting pipeline. The discharge port at the top of the gas-liquid separator is connected with the feed inlet of the cooling heat exchanger 12 through a pipeline, and the discharge port of the cooling heat exchanger 12 is connected with a condensate collecting tank through a pipeline.
All levels of crystallization kettles 6 are provided with a crystallization kettle feeding port and a crystallization kettle discharging port, a material outlet 403 at the bottom of the distillation concentration kettle is connected with a first level crystallization kettle feeding port 601 through a pipeline, a material transferring pump and a cooler 5 are connected to a connecting pipeline connection, and a next level crystallization kettle discharging port 602 is connected with a previous level crystallization kettle feeding port 601. The top of the distillation concentration kettle is provided with a mother liquor circulating feed inlet which is connected with a mother liquor collecting tank 11 through a pipeline a15, the mother liquor collecting tank 11 leads collected mother liquor into the distillation concentration kettle to recycle the mother liquor, and the last-stage crystallization kettle 6 is provided with a circulating water jacket layer to control the temperature in the last-stage crystallization kettle 6.
The discharge port 602 of the last-stage crystallization kettle is connected with a centrifuge 9; and a discharge hole of the centrifugal machine 9 is respectively connected with the mother liquor collecting tank 11 and the finished product tank.
The crystallization kettle 6 can be made of any one of enamel, glass lining, steel lining plastic and stainless steel. The discharge port 602 of the crystallization kettle is a wide-opening hopper-type discharge port. The crystallization kettle 6 is provided with a rod-shaped dentate stirring device 603, and each rod-shaped stirring tooth 604 on the stirring device 603 is staggered from top to bottom along the direction vertical to the stirring rod and is connected with the stirring rod in a seamless way. The crystallization kettle 6 is provided with a liquid level meter 605 or weighing unit, and a one-to-one PLC interlocking device is established between each liquid level meter 605 or weighing unit and the feeding valve at the top inlet position and the discharging valve at the bottom discharging buckle position of the corresponding crystallization kettle 6.
In the embodiment of the method, the first step,
the device is used for preparing amino trimethylene phosphonic acid or hydroxy ethylidene diphosphonic acid liquid, four groups of crystallization kettles are used, the 1-4-level crystallization kettles and the corresponding stirring devices are all made of stainless steel, the specifications of the 1-3-level crystallization kettles are V =200m for carrying out heavy year, and DN =1200 mm. All be equipped with the agitating unit that length is about 3.5m in the 1~4 level crystallization cauldron, the last bar type tooth that is equipped with length of agitating unit is 45cm, and each bar-shaped stirring tooth is along perpendicular puddler direction top-down to be crisscross distribution around, and seamless connection between with the puddler.
The crystallization kettles of 1-4 levels are all provided with liquid level meters, a one-to-one PLC automatic interlocking device is built between each liquid level meter and the corresponding top feeding valve and bottom discharging valve of the crystallization kettle, when the material liquid level in each crystallization kettle is more than or equal to 3/4 of the volume of the crystallization kettle, the top feeding valve is automatically closed, the bottom discharging valve is opened, and the solid-liquid mixed material automatically enters the next-level crystallization kettle from a wide-opening hopper type discharging opening 602 at the bottom of the crystallization kettle; when the material liquid level in each stage of crystallization kettle reaches 1/4 that the crystallization kettle is smaller than the volume of the crystallization kettle, the bottom discharge valve is automatically closed, and the top feed valve is opened;
the natural cooling temperature range when the materials in the 1-4-level crystallization kettle reach the set automatic material transferring volume is respectively as follows: 50-60 ℃, 45-50 ℃, 35-40 ℃ and 30-35 ℃.
The discharge hole 304 of the top of the gas-liquid separator is connected with the feed hole of the cooling heat exchanger through a pipeline, the discharge hole of the cooling heat exchanger is connected with a condensate collecting tank 13 through a pipeline, and the condensate is circularly used as process water for the production line of the amino trimethylene phosphonic acid or hydroxy ethylidene diphosphonic acid liquid product.
The continuous production device for the organic phosphine crystals comprises the following specific working processes:
products from a liquid production line of amino trimethylene phosphonic acid or hydroxy ethylidene diphosphonic acid enter a liquid product tank 1 made of enamel materials with the volume of 1000m through a liquid product tank feed inlet 101, the liquid products are continuously pumped into a YKB type shell and tube graphite heater 2 with the heat exchange area of 500 square meters at a liquid product tank discharge outlet 102 through a material transfer pump according to a set flow rate to be preheated to 75 +/-5 ℃, the preheated materials are preliminarily separated by gravity settling through a gas-liquid separator 3 to remove low boiling point substances such as hydrogen chloride and the like and a small amount of water vapor in the raw materials, high boiling point liquid materials enter a distillation concentration kettle 4 in a stirring state through a concentration distillation kettle top feed inlet 401 from a gas-liquid separator bottom discharge outlet 302, the materials pumped into the distillation concentration kettle are subjected to rapid negative pressure external evaporation concentration through interlayer vapor, when the concentration of a material system in the concentration distillation kettle is more than 70 percent, a distillation concentration kettle bottom material discharge outlet 403 discharge valve is opened to continuously pump the materials into a heat exchange stone with the heat exchange area of 200 The ink cooler 5 is used for naturally cooling and crystallizing supersaturated materials flowing out from the cooling and discharging port 502 at the temperature of about 60-70 ℃ after heat exchange through a 1-4-grade crystallization kettle in sequence, cooling to 20 +/-2 ℃ through circulating cooling in a fourth-grade crystallization kettle, fully crystallizing, then feeding the supersaturated materials into an automatic discharging centrifuge 9 from a discharging port of the fourth-grade crystallization kettle, performing centrifugal drying treatment, and packaging amino trimethylene phosphonic acid crystals or hydroxy ethylidene diphosphonic acid crystals into finished products by a filling machine 10, wherein the activity content of the finished products is more than or equal to 95%. Mother liquor separated by a centrifuge enters a mother liquor collecting tank 11 for collection, and the mother liquor is continuously pumped into an evaporation concentration kettle 4 for recycling until the chroma is more than 180Hazen, and can be diluted to be used as a compound phosphorus-containing scale and corrosion inhibitor monomer.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (9)
1. A continuous production device for organic phosphine crystals is characterized by comprising a liquid product tank (1), a heater, a gas-liquid separator, a distillation and concentration kettle, a 1-n-stage crystallization kettle (6) and a centrifugal machine (9), wherein n is more than or equal to 2 and less than or equal to 8; a liquid product tank feeding port (101) is directly connected with a liquid production line, a liquid product tank discharging port (102) is connected with a heater feeding port (201) through a pipeline, and a heater discharging port (202) is connected with a gas-liquid separator bottom feeding port A (301); the distillation concentration kettle is provided with a reaction kettle jacket and a paddle stirrer, wherein the reaction kettle jacket is provided with an interlayer steam inlet (404) and an interlayer steam condensate outlet (405), the distillation concentration kettle is provided with a distillation concentration kettle top inlet (401), a distillation concentration kettle top outlet (402) and a distillation concentration kettle bottom material outlet (403), the distillation concentration kettle top inlet (401) is connected with a gas-liquid separator bottom discharge port (302) through a pipeline, the distillation concentration kettle top outlet (402) is connected with a gas-liquid separator bottom feed port B (303), each crystallization kettle (6) is provided with a crystallization kettle feed port and a crystallization kettle discharge port, the distillation concentration kettle bottom material outlet (403) is connected with a first-stage crystallization kettle feed port (601) through a pipeline, and a next-stage crystallization kettle discharge port (602) is connected with a last-stage crystallization kettle feed port (601); a discharge port (602) of the last-stage crystallization kettle is connected with a centrifuge (9); and a discharge hole of the centrifugal machine (9) is respectively connected with the mother liquor collecting tank (11) and the finished product tank.
2. The continuous production device of organophosphine crystals according to claim 1, wherein a valve and a material transfer pump are connected in series on a connecting line between the discharge port (102) of the liquid product tank and the feed port (201) of the heater; a negative pressure pump (14) is arranged on a connecting pipeline between an outlet (402) at the top of the distillation concentration kettle and a feed inlet B (303) at the bottom of the gas-liquid separator; the material outlet (403) at the bottom of the distillation concentration kettle is connected with the feeding hole (601) of the first-stage crystallization kettle through a pipeline, and a material transferring pump and a cooler (5) are connected with the pipeline.
3. The continuous production device of organophosphine crystals according to claim 1 or 2, wherein the material of the crystallization kettle (6) can be any one of an enamel reaction kettle, a glass lining kettle, a steel lining plastic reaction kettle, and a stainless steel reaction kettle.
4. The continuous production device of organophosphine crystals according to claim 1 or 2, wherein the discharge port (602) of the crystallization kettle is a wide-mouth hopper-type discharge port.
5. The continuous production apparatus of organophosphine crystals according to claim 1 or 2, wherein the crystallization kettles (6) are all provided with rod-shaped toothed stirring devices (603), and each rod-shaped stirring tooth (604) on the stirring devices (603) is staggered from top to bottom along the direction vertical to the stirring rod and is connected with the stirring rod without seam.
6. The continuous production device of organophosphine crystals according to claim 1, wherein the crystallization kettles (6) are equipped with level meters (605) or weighing units, and a one-to-one PLC interlock is established between each level meter (605) or weighing unit and the corresponding feeding valve at the top inlet position and the discharging valve at the bottom discharging buckle position of the crystallization kettle (6).
7. The continuous production device of organophosphine crystals according to claim 1, wherein a mother liquor circulating feed port is arranged at the top of the distillation concentration kettle and is connected with a mother liquor collecting tank (11) through a pipeline a (15), the mother liquor collecting tank (11) feeds the collected mother liquor into the distillation concentration kettle for recycling the mother liquor, and the nth-stage crystallization kettle is provided with a circulating water jacket layer for controlling the temperature in the nth-stage crystallization kettle.
8. The continuous production device of organophosphine crystals according to claim 1, wherein the discharge port at the top of the gas-liquid separator is connected with the feed port of the cooling heat exchanger (12) through a pipeline, and the discharge port of the cooling heat exchanger (12) is connected with the condensate collecting tank through a pipeline.
9. The apparatus for continuously producing organophosphine crystals according to claim 1, wherein the apparatus is suitable for continuously producing organophosphine crystal products such as aminotrimethylene, hydroxyethylidene diphosphonic acid, etc.
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| CN201921594694.0U CN210595870U (en) | 2019-09-24 | 2019-09-24 | Continuous production device for organic phosphine crystals |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021073198A1 (en) * | 2019-10-17 | 2021-04-22 | 山东泰和水处理科技股份有限公司 | Continuous production method for amino trimethylene phosphonic acid crystal |
| WO2021073199A1 (en) * | 2019-10-17 | 2021-04-22 | 山东泰和水处理科技股份有限公司 | Continuous production method for hydroxyethylene diphosphonic acid crystals |
-
2019
- 2019-09-24 CN CN201921594694.0U patent/CN210595870U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021073198A1 (en) * | 2019-10-17 | 2021-04-22 | 山东泰和水处理科技股份有限公司 | Continuous production method for amino trimethylene phosphonic acid crystal |
| WO2021073199A1 (en) * | 2019-10-17 | 2021-04-22 | 山东泰和水处理科技股份有限公司 | Continuous production method for hydroxyethylene diphosphonic acid crystals |
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Address after: No.1, Shiliquan East Road, Shizhong District, Zaozhuang City, Shandong Province 277100 Patentee after: Shandong Taihe Technology Co.,Ltd. Address before: No.1, Shiliquan East Road, Shizhong District, Zaozhuang City, Shandong Province 277100 Patentee before: SHANDONG TAIHE WATER TREATMENT TECHNOLOGIES Co.,Ltd. |
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