CN214131576U

CN214131576U - Preparation equipment of hydroxyl ethylidene diphosphate tetrasodium solid product

Info

Publication number: CN214131576U
Application number: CN202023245845.7U
Authority: CN
Inventors: 张庆龙; 段丽菊; 石志付; 赵一杰
Original assignee: Shandong Huayou Water Processing Technology Co ltd
Current assignee: Shandong Huayou Water Processing Technology Co ltd
Priority date: 2020-12-28
Filing date: 2020-12-28
Publication date: 2021-09-07
Anticipated expiration: 2030-12-28

Abstract

The utility model discloses a preparation equipment of hydroxyl ethylidene diphosphate tetrasodium solid product. A preparation device of a solid product of hydroxyethylidene tetrasodium diphosphate comprises an HEDP aqueous solution storage tank, an HEDP aqueous solution conveying device, a sodium hydroxide solution storage tank, a sodium hydroxide solution conveying device, an HEDP aqueous solution and sodium hydroxide solution mixed reaction device, a feed liquid drying device of a reaction product of a solid target product of hydroxyethylidene tetrasodium diphosphate obtained after the reaction of HEDP and sodium hydroxide is completed, and a cleaning device of the HEDP aqueous solution and sodium hydroxide solution mixed reaction device. The crystallization yield of the solid organic phosphonate (HEDP. Na4) is improved, the effective components in the HEDP aqueous solution and the sodium hydroxide solution are completely converted into the hydroxyethylidene tetrasodium diphosphate solid product, and the primary yield of the solid organic phosphonate (HEDP. Na4) is improved by 3 times compared with that of the solid organic phosphonate (HEDP. Na4) in the prior art; the quality of the finished product of the solid sodium hydroxide ethylidene diphosphate is stabilized.

Description

Preparation equipment of hydroxyl ethylidene diphosphate tetrasodium solid product

Technical Field

The utility model relates to a field is made in the production of water treatment chemicals, belongs to a water quality stabilizer's preparation equipment, especially relates to a preparation equipment of hydroxyl ethylidene diphosphate tetrasodium solid product.

Background

The solid product of the etidronate tetrasodium is solid organic phosphonate (HEDP. Na4), and the solid product of the etidronate tetrasodium is white powder, is easy to dissolve in water, does not absorb moisture, is convenient to transport, and is suitable for being used under severe cold conditions. HEDP Na4 belongs to organic phosphonate scale and corrosion inhibitor, can form stable complex with iron, copper, zinc and other metal ions, can dissolve oxide on the metal surface, and still has good corrosion and scale inhibition effects at 250 ℃. The solid product of the hydroxyl ethylidene diphosphate tetrasodium is widely applied to scale inhibition and corrosion inhibition of industrial circulating cooling water such as electric power, chemical engineering, metallurgy, chemical fertilizer and the like, low-pressure boilers, oilfield water injection and oil pipelines; the solid product of hydroxy ethylidene diphosphate can be used as metal and nonmetal cleaning agent, peroxide stabilizer and color fixing agent in printing and dyeing industry, cyanide-free electroplating complexing agent, daily chemical additive and hydrogen peroxide stabilizer in light textile industry. The existing production method of the solid product of the hydroxyethylidene diphosphate tetrasodium is that liquid HEDP is added with sodium (potassium) hydroxide in a reaction kettle to react into HEDP. Na (K) x salt, wherein x can be 2 or 4, then the reaction kettle is heated to vaporize moisture, the temperature is reduced after the moisture is proper to crystallize out solid, a centrifuge is used for separating out mother liquor, and the solid is dried to obtain a finished product. The yield of the first crystallization of the solid organic phosphonate (HEDP. Na4) produced in the way is about 30 percent, the mother liquor is large in amount, and the yield is low; the mother liquor needs to be recycled for many times, and is repeatedly heated and cooled, so that the energy consumption is high; the solubility of Na4 is great along with temperature variation, and in centrifugation, centrifuge makes the feed liquid rotate at a high speed, and moisture vaporizes rapidly, and the material sharply reduces the temperature, and the material in the centrifuge and a large amount of micrite granule in the hydrops groove of centrifuge bottom separate out, and the solid-liquid separation is difficult to appear, and hydrops groove blocks up, needs frequent hot mother liquor with the heating to wash centrifuge and washing mother liquor groove, has influenced the productivity, also does not benefit to the environmental protection. The method disclosed in the chinese patent 201310057644.X is to stir the HEDP liquid and the alkali in a reaction kettle to form solid particles or powder, and then send the dried finished product. The method requires expensive equipment and high stirring power; the obtained material in the reaction kettle has poor fluidity and difficult discharging; intermittent reaction, large quality fluctuation of finished products and low productivity. How to improve the crystallization yield of the solid organic phosphonate (HEDP. Na4), improve the yield of the solid sodium hydroxy ethylidene diphosphate product, protect the environment and cancel the solid-liquid separation process; how to reduce the manufacturing cost and the operation cost of equipment and stabilize the quality of finished products of hydroxyl ethylidene diphosphate tetrasodium solid products is a technical problem to be solved.

SUMMERY OF THE UTILITY MODEL

The utility model aims to solve the technical problem of providing a preparation device of a solid product of hydroxyl ethylidene diphosphate tetrasodium. The preparation equipment of the solid product of the hydroxyethylidene diphosphate tetrasodium can improve the crystallization yield of the solid organic phosphonate (HEDP. Na4), improve the yield of the solid product of the hydroxyethylidene diphosphate tetrasodium, protect the environment and cancel the solid-liquid separation process; and the equipment manufacturing cost and the equipment running cost can be reduced, and the quality of finished products of the hydroxyl ethylidene diphosphate tetrasodium solid products is stabilized.

The utility model provides a technical scheme that its technical problem adopted is: a preparation device of a solid product of hydroxyl ethylidene diphosphate tetrasodium, which is characterized in that: the device comprises an HEDP aqueous solution storage tank, an HEDP aqueous solution conveying device, a sodium hydroxide solution storage tank, a sodium hydroxide solution conveying device, an HEDP aqueous solution and sodium hydroxide solution mixed reaction device, a device for drying feed liquid of a reaction product of a solid target product of the hydroxyl ethylidene diphosphate tetrasodium obtained after the reaction of the HEDP and the sodium hydroxide is completed, a cleaning device of the HEDP aqueous solution and sodium hydroxide solution mixed reaction device and a control device;

the HEDP aqueous solution and sodium hydroxide solution mixed reaction device comprises a tubular mixed reactor and a tubular mixed reactor mounting bracket, wherein the tubular mixed reactor mounting bracket is arranged at the middle position of a steel-concrete platform, the tubular mixed reactor is arranged on the top surface of the tubular mixed reactor mounting bracket, the tubular mixed reactor arranged on the top surface of the tubular mixed reactor mounting bracket is provided with a tubular reaction section, a tubular reaction section joint section and a tubular reactant spraying section, the tubular reactant spraying section is L-shaped, a granulation spray head is arranged on the end part of the vertical part of the L-shaped tubular reactant spraying section in a threaded manner, and two ends of the tubular reaction section of the tubular mixed reactor are respectively fixedly connected by using a flange, the tubular reaction section joint section and the end part of the horizontal part of the tubular reactant spraying section; the middle section of a tubular reaction section of the tubular mixed reactor is a part with a thickened inner wall, at least 3 inwards concave annular grooves with arc-shaped vertical sections are sequentially arranged on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section, the left notch of the outwards concave annular groove with the left most left vertical section on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is connected with the cambered surface of the left inner wall of the tubular reaction section which is integrally formed, the right notch of the inwards concave annular groove with the right most right vertical section on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is connected with the cambered surface of the right inner wall of the tubular reaction section which is integrally formed, and the thickened thickness of the thickened inner wall of the middle section of the tubular reaction section is 0.3-0.5 mm; the length of the tubular reaction section of the tubular mixed reactor is 6-6.5 meters, and the inner diameter of the parts at two sides of the thickened middle section of the inner wall of the tubular reaction section is 4.5-5 mm;

the HEDP aqueous solution conveying device comprises an HEDP aqueous solution pump and an HEDP aqueous solution conveying pipeline, the HEDP aqueous solution conveying pipeline is provided with a vertical part and a horizontal part which are integrally formed, the end part of the vertical part of the HEDP aqueous solution conveying pipeline is communicated, sealed and fixedly connected with an HEDP aqueous solution storage tank, the end part of the horizontal part is communicated, sealed and fixedly connected with an HEDP aqueous solution inlet arranged on a joint section of a tubular reaction section of the tubular mixing reactor, an HEDP aqueous solution filter is arranged on the part, close to the HEDP aqueous solution storage tank, of the vertical part of the HEDP aqueous solution conveying pipeline on the upper side of the HEDP aqueous solution filter, the HEDP aqueous solution pump is arranged on the vertical part of the HEDP aqueous solution conveying pipeline on the upper side of the HEDP aqueous solution pump, and an HEDP aqueous solution flow meter is arranged on the vertical part of the HEDP aqueous solution conveying pipeline on the upper side of the HEDP aqueous solution pump; the device also comprises an HEDP aqueous solution backflow pipeline, wherein the HEDP aqueous solution backflow pipeline is provided with a vertical part and a transverse part which are integrally formed, the end part of the vertical part of the HEDP aqueous solution backflow pipeline is communicated, sealed and fixedly connected with an HEDP aqueous solution storage tank, the end part of the transverse part is communicated, sealed and fixedly connected with a pipeline section part of the vertical part of an HEDP aqueous solution conveying pipeline between an HEDP aqueous solution flowmeter and an HEDP feed liquid pump, and an A electromagnetic valve is arranged on the transverse part of the HEDP aqueous solution backflow pipeline;

the sodium hydroxide solution conveying device comprises a sodium hydroxide solution feed pump, the device comprises a sodium hydroxide solution conveying pipeline, a sodium hydroxide solution conveying pipeline and a liquid level meter, wherein the sodium hydroxide solution conveying pipeline is provided with a vertical part and a horizontal part which are integrally formed, the end part of the vertical part of the sodium hydroxide solution conveying pipeline is communicated, sealed and fixedly connected with a sodium hydroxide solution storage tank, the end part of the horizontal part is communicated, sealed and fixedly connected with a sodium hydroxide solution inlet arranged on a tubular reaction section joint section of a tubular mixing reactor, a sodium hydroxide solution filter is arranged on the part, close to the sodium hydroxide solution storage tank, of the vertical part of the sodium hydroxide solution conveying pipeline, a sodium hydroxide solution liquid pump is arranged on the vertical part of the sodium hydroxide solution conveying pipeline on the upper side of the sodium hydroxide solution filter, and a sodium hydroxide solution flow meter is arranged on the vertical part of the sodium hydroxide solution; the system also comprises a sodium hydroxide solution backflow pipeline, wherein the sodium hydroxide solution backflow pipeline is provided with a vertical part and a transverse part which are integrally formed, the end part of the vertical part of the sodium hydroxide solution backflow pipeline is communicated, sealed and fixedly connected with a sodium hydroxide solution storage tank, the end part of the transverse part is communicated, sealed and fixedly connected with a pipeline section part of the vertical part of a sodium hydroxide solution conveying pipeline between a sodium hydroxide solution flowmeter and a sodium hydroxide solution feed liquid pump, and a B electromagnetic valve is arranged on the transverse part of the sodium hydroxide solution backflow pipeline;

the cleaning device of the HEDP water solution and sodium hydroxide solution mixed reaction device comprises a cleaning water storage tank, a cleaning water pump and a cleaning water pipeline, wherein the cleaning water pipeline is provided with an integrally formed vertical part and a horizontal part, the end part of the vertical part of the cleaning water pipeline is communicated, sealed and fixedly connected with the cleaning water storage tank, the end part of the horizontal part is communicated, sealed and fixedly connected with a cleaning water pipeline connecting port arranged on a tubular reaction section joint section of the tubular mixed reactor, the cleaning water pump is arranged on the part, close to the cleaning water storage tank, of the vertical part of the cleaning water pipeline, the cleaning water reflux pipeline is provided with an integrally formed vertical part and a horizontal part, the end part of the vertical part of the cleaning water reflux pipeline is communicated, sealed and fixedly connected with the cleaning water storage tank, and the end part of the horizontal part is communicated, sealed and fixedly connected with the pipeline section, the transverse part of the cleaning water backflow pipeline is provided with a C electromagnetic valve;

the feed liquid drying device for the reaction product of the hydroxyethylidene tetrasodium diphosphate solid target product obtained after the reaction of the HEDP and the sodium hydroxide is completed comprises a drying tower, a fan, an air suction pipeline, a heat exchanger and a hot air conveying pipe, the drying tower is arranged on a steel-concrete platform on the right side of the mounting bracket of the tubular mixing reactor by using a drying tower base, the part of the tubular reaction section of the tubular mixing reactor arranged on the top surface of the mounting bracket of the tubular mixing reactor and the tubular reactant spraying section of the tubular mixing reactor provided with a granulating nozzle penetrate through a through hole arranged on the upper part of the left side of the drying tower and extend into the drying tower and are fixedly arranged on the through hole arranged on the upper part of the left side of the drying tower in a sealing way, the vertical axis of the granulation nozzle of the reaction section of the tubular mixed reactor, the tubular reactant spraying section provided with the granulation nozzle, and the vertical axis of the drying tower extend into the drying tower and are fixedly arranged on the through hole at the upper part of the left side of the drying tower in a sealing way; the heat exchanger is arranged on a steel-concrete platform at the lower part of the right side of the drying tower by using a heat exchanger mounting seat, and a hot air conveying pipe arranged on the heat exchanger is communicated, sealed and fixedly connected with the lower part of the right side wall of the drying tower; the air suction pipeline is fixedly connected with the upper end part of the right side wall of the drying tower in a penetrating and sealing way, the right end part of the air suction pipeline is provided with a fan, and an air exhaust pipe is arranged on an air exhaust port of the fan; the air suction pipeline on the left side of the fan is also provided with a dust remover; the inner surface of the bottom of the drying tower is an inclined plane inclined towards the left side, a discharge port is arranged at the position, close to the inner surface of the inclined plane inclined towards the left side, of the bottom of the left side of the bottom of the drying tower, and a star-shaped discharger is mounted at the discharge port arranged at the bottom of the left side of the bottom of the drying tower through a mounting seat.

The granulation sprayer, the drying tower, the heat exchanger, the dust remover and the star-shaped discharger which are arranged at the tubular reactant spraying section of the reaction section of the tubular mixed reactor adopt the prior art; the control device is a DCS control cabinet, and the DCS control cabinet adopts the prior art; the HEDP feed liquid pump, the electromagnetic valve A, the sodium hydroxide solution feed liquid pump, the electromagnetic valve B, the cleaning water pump, the electromagnetic valve C, the fan, the dust remover, the heat exchanger and the star-shaped discharger are respectively electrically connected with and controlled by the DCS control cabinet.

Use the utility model discloses the process that preparation equipment of the solid product of four sodium hydroxide ethylidene diphosphate prepared a solid product of four sodium hydroxide ethylidene diphosphate is:

the solid product of the hydroxyl ethylidene diphosphate tetrasodium is prepared by reacting an HEDP aqueous solution with a sodium hydroxide solution, wherein the molar ratio of the HEDP to the sodium hydroxide is 1: 4.02 to 4.08, preferably the molar ratio of HEDP reacted with sodium hydroxide is 1: 4.03; the preparation process of the solid product of the hydroxyl ethylidene diphosphate tetrasodium comprises the following steps:

A. according to the molar ratio of HEDP to sodium hydroxide reaction of 1: 4.02-4.08 preparing the HEDP aqueous solution and the sodium hydroxide solution correspondingly, wherein the volume ratio of the HEDP aqueous solution to the sodium hydroxide solution prepared correspondingly is 1: 0.78-0.81, the concentration of the HEDP aqueous solution is 60% (weight percentage), and the concentration of the sodium hydroxide solution is 40% (weight percentage); feeding the HEDP aqueous solution and the sodium hydroxide solution which are prepared correspondingly into an HEDP aqueous solution storage tank and a sodium hydroxide solution storage tank for later use;

B. starting a heat exchanger, wherein the temperature of hot air output by a hot air conveying pipe arranged on the heat exchanger is 55-60 ℃; starting a fan, and rising hot air output by a hot air delivery pipe with the temperature of 55-60 ℃ along a drying tower;

C. starting an HEDP feed liquid pump, filtering an HEDP aqueous solution by an HEDP aqueous solution filter, metering the HEDP aqueous solution by an HEDP aqueous solution flowmeter, and conveying the HEDP aqueous solution to a tubular reaction section joint section of the tubular mixing reactor along an HEDP aqueous solution conveying pipeline and through an HEDP aqueous solution input port on the tubular reaction section joint section which is fixedly connected with the HEDP aqueous solution conveying pipeline in a penetrating and sealing manner through the transverse part end part of the HEDP aqueous solution conveying pipeline; simultaneously starting a sodium hydroxide solution feed pump, filtering the sodium hydroxide solution by a sodium hydroxide solution filter, metering by a sodium hydroxide solution flowmeter, and conveying the sodium hydroxide solution to a tubular reaction section joint section of the tubular mixing reactor along a sodium hydroxide solution conveying pipeline and through a sodium hydroxide solution inlet on the tubular reaction section joint section which is fixedly connected with the sodium hydroxide solution conveying pipeline in a penetrating and sealing manner through the transverse part end of the sodium hydroxide solution conveying pipeline; HEDP aqueous solution and sodium hydroxide solution which are simultaneously conveyed to a tubular reaction section joint section of a tubular mixed reactor are mixed and enter a tubular reaction section of the tubular mixed reactor, HEDP entering the tubular reaction section of the tubular mixed reactor and sodium hydroxide are reacted to obtain reaction product feed liquid of a solid target product of hydroxyethylidene diphosphate, the reaction product feed liquid enters a tubular reactant ejection section provided with a granulation nozzle and is ejected out by the granulation nozzle to atomize the reaction product feed liquid of the solid target product of hydroxyethylidene diphosphate, the reaction of HEDP and sodium hydroxide entering the tubular reaction section of the tubular mixed reactor belongs to exothermic reaction, the temperature of the reaction product feed liquid of the solid target product of the atomized solid target product of the hydroxyethylidene diphosphate ejected by the granulation nozzle and the tubular reactant ejection section provided with the granulation nozzle is 115-130 ℃, and the temperature of the reaction product feed liquid of the solid target product of the atomized solid target product of the hydroxyethylidene diphosphate ejected by the granulation nozzle and the tubular reactant ejection section provided with the granulation nozzle is ejected by the granulation nozzle The feed liquid is contacted with the rising hot air with the temperature of 55-60 ℃ in the drying tower due to the gravity reduction, the moisture is vaporized and enters a gas phase, the finished product of the hydroxyl ethylidene diphosphate tetrasodium solid powder is obtained after drying, the hydroxyl ethylidene diphosphate tetrasodium solid powder falls to the bottom of the drying tower and slides to a discharge port along the inclined inner surface which inclines leftwards at the bottom of the drying tower, the inclined inner surface is pulled out by a star-shaped discharger and enters the next processing procedure, and the waste gas in the drying tower is discharged after dust removal by a dust remover and reaches the standard through an exhaust pipe;

D. and (3) equipment shutdown procedures: sequentially shutting down an HEDP material liquid pump and a sodium hydroxide solution material liquid pump, starting a cleaning water pump, conveying cleaning water to the tubular mixing reactor along a cleaning water conveying pipeline, and sequentially cleaning a tubular reaction section joint section, a tubular reaction section and a tubular reactant spraying section provided with a granulation spray head of the tubular mixing reactor for 10-15 seconds; sequentially shutting down the heat exchanger, the dust remover and the fan in sequence, and shutting down the equipment;

the temperature of the HEDP aqueous solution is 10-50 ℃, and the temperature of the sodium hydroxide solution is 10-50 ℃;

the reaction pressure of the mixed reactor is 0.1MPa-0.7MPa, and the reaction time is 2-8S;

the outlet pressure of the HEDP feed liquid pump and the outlet pressure of the sodium hydroxide solution feed liquid pump are both 0.4-0.45 MPa;

the preferred technical scheme is as follows: the temperature of the HEDP aqueous solution is 25-30 ℃, and the temperature of the sodium hydroxide solution is 25-30 ℃; the reaction pressure of the mixed reactor is 0.3MPa-0.5MPa, and the reaction time is 3-5S; the pump outlet pressure of the HEDP feed liquid pump and the pump outlet pressure of the sodium hydroxide solution feed liquid pump are both 0.42 MPa.

The utility model has the advantages that: because the utility model is provided with an HEDP aqueous solution storage tank, an HEDP aqueous solution conveying device, a sodium hydroxide solution storage tank, a sodium hydroxide solution conveying device, a HEDP aqueous solution and sodium hydroxide solution mixed reaction device, a hydroxyl ethylidene diphosphonic acid tetrasodium solid target product reaction product feed liquid drying device obtained after the HEDP and sodium hydroxide complete reaction, a cleaning device of the HEDP aqueous solution and sodium hydroxide solution mixed reaction device, and a control device; use the utility model discloses the preparation equipment of the solid product of four sodium hydroxide ethylidene diphosphate prepares a solid product preparation process of four sodium hydroxide ethylidene diphosphate: the solid product of the hydroxyl ethylidene diphosphate tetrasodium is prepared by the reaction of an HEDP aqueous solution and a sodium hydroxide solution, wherein the molar ratio of the HEDP to the sodium hydroxide is 1: 4.02-4.08; according to the molar ratio of HEDP to sodium hydroxide reaction of 1: 4.02-4.08 preparing the HEDP aqueous solution and the sodium hydroxide solution correspondingly, wherein the volume ratio of the HEDP aqueous solution to the sodium hydroxide solution prepared correspondingly is 1: 0.78-0.81, the concentration of HEDP aqueous solution is 60% (weight percentage), the concentration of sodium hydroxide solution is 40% (weight percentage); the temperature of the HEDP aqueous solution is 10-50 ℃, and the temperature of the sodium hydroxide solution is 10-50 ℃; the reaction pressure of the mixed reactor is 0.1MPa-0.7MPa, and the reaction time is 2-8S; the pump outlet pressure of the HEDP feed liquid pump and the pump outlet pressure of the sodium hydroxide solution feed liquid pump are both 0.4-0.45 MPa. The utility model provides high solid organic phosphonate (HEDP Na4) crystallization yield, the utility model discloses effective component in HEDP aqueous solution, the sodium hydroxide solution converts into hydroxyl ethylidene diphosphate tetrasodium solid product completely, improves 3 times for prior art solid organic phosphonate (HEDP Na4) primary yield, has improved hydroxyl ethylidene diphosphate tetrasodium solid product output, has protected the environment, cancels the solid-liquid separation process; also reduces the equipment manufacturing cost and the equipment operating cost, and stabilizes the quality of the finished product of the solid sodium hydroxide ethylidene diphosphate.

The utility model discloses still have following innovation characteristics:

firstly, the middle section of the tubular reaction section of the tubular mixed reactor is a part with thickened inner wall, at least 3 inwards concave ring grooves with arc-shaped vertical cross sections are sequentially arranged on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section, the leftmost vertical cross section on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is an arc-shaped inwards concave ring groove left side notch and is connected with the arc surface of the integrally formed inner wall of the left side of the tubular reaction section, the rightmost vertical cross section on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is an arc-shaped inwards concave ring groove right side notch and is connected with the arc surface of the integrally formed inner wall of the right side of the tubular reaction section, and the thickened inner wall of the middle section of the tubular reaction section is 0.3-0.5 mm; the length of the tubular reaction section of the tubular mixed reactor is 6-6.5 m, and the inner diameter of the thickened part at the two sides of the middle section of the inner wall of the tubular reaction section is 4.5-5 mm. The pipe diameter of the middle section of the tubular reaction section of the tubular mixed reactor is large and small, the inner pipe wall of the middle section of the tubular reaction section of the vertical cross section is a curved wave line, when HEDP aqueous solution and sodium hydroxide solution which are simultaneously conveyed to the joint section of the tubular reaction section of the tubular mixed reactor are mixed and enter the tubular reaction section of the tubular mixed reactor, the mixed solution of the HEDP aqueous solution and the sodium hydroxide solution which are conveyed to the middle section of the tubular reaction section of the vertical cross section tubular reaction section of the tubular reaction section is forced to rapidly and continuously change the running direction along the curved wave line of the inner pipe wall of the middle section of the tubular reaction section, high-speed turbulence is formed, sufficient mixing is realized, and the HEDP entering the tubular reaction section of the tubular mixed reactor can completely react with the sodium hydroxide, obtaining the reaction product liquid of the solid target product of the hydroxyethylidene diphosphate, wherein the reaction product liquid of the solid target product of the hydroxyethylidene diphosphate cannot be supersaturated to separate out solid to block equipment; the effective components of the HEDP aqueous solution and the sodium hydroxide solution are completely converted into a solid product of the hydroxyethylidene diphosphate tetrasodium, and the primary yield of the solid product is improved by 3 times compared with that of the solid organic phosphonate (HEDP. Na4) in the prior art;

secondly, the concentration of the reaction material liquid after the reaction of the HEDP entering the tubular reaction section of the tubular mixed reactor and the sodium hydroxide is finished greatly exceeds the solubility of the HEDP; the normal temperature saturation concentration of HEDP. Na4 is 22.5-23.0%, the reaction material liquid concentration after the HEDP entering the tubular reaction section of the tubular mixed reactor and the sodium hydroxide are reacted is 45-46%, because the reaction time of the HEDP entering the tubular reaction section of the tubular mixed reactor and the sodium hydroxide in the reaction section of the mixed reactor is very short, 2-8S, and the reaction pressure is 0.1MPa-0.7 MPa; HEDP entering a tubular reaction section of the tubular mixing reactor can completely react with sodium hydroxide to obtain a reaction product feed liquid of a solid target product of the hydroxyethylidene diphosphate, and the reaction product feed liquid of the solid target product of the hydroxyethylidene diphosphate can not separate out solid to block equipment due to supersaturation; the liquid of the reaction product of the solid target product of the hydroxyethylidene diphosphate is sprayed out of the tubular mixing reactor in a fluid atomization state through the granulating nozzle, so that the reaction can be carried out under high concentration and low water content, the continuous production is realized, and the steam and power consumption are saved; conditions are also created for obtaining a solid finished product of the hydroxyethylidene diphosphate tetrasodium by a spray drying method;

thirdly, the utility model simultaneously conveys HEDP aqueous solution of the tubular reaction section joint section of the tubular mixed reactor and sodium hydroxide solution to mix and enter the tubular reaction section of the tubular mixed reactor, the HEDP and the sodium hydroxide entering the tubular reaction section of the tubular mixed reactor enter the tubular reactant spraying section provided with the granulation nozzle after finishing reaction and spray atomized tetra-sodium hydroxy ethylidene diphosphate solid target product reaction product feed liquid by the granulation nozzle, the reaction of the HEDP and the sodium hydroxide entering the tubular reaction section of the tubular mixed reactor belongs to exothermic reaction, the temperature of the atomized tetra-sodium hydroxy ethylidene diphosphate solid target product reaction product feed liquid sprayed by the granulation nozzle leaving the mixed reactor is 115-130 ℃, the atomized tetra-sodium hydroxy ethylidene diphosphate solid target product reaction product feed liquid rapidly vaporizes partial moisture due to pressure reduction after leaving the mixed reactor, simultaneously under the effect of dry hot air of drying tower, atomizing hydroxyl ethylidene diphosphate tetrasodium solid target product reaction product feed liquid is at the further evaporation moisture of decline in-process, obtains promptly at the drying tower bottom the utility model discloses hydroxyl ethylidene diphosphate tetrasodium solid product. The utility model makes full use of the reaction heat of the materials and saves the energy.

See the utility model discloses the solid product quality detection table of hydroxyl ethylidene diphosphate tetrasodium:

item	Standard of merit	The result of the detection
			pH value (1% aqueous solution)	10.5-12.0	11.53
Loss on drying(％)	≤15	11.1
			Effective content (% by HEDP)	≥56.0	57.7
Na4 content (%)	≥80.0	82.3

Drawings

The present invention will be further explained with reference to the drawings and examples;

FIG. 1 is a schematic structural view of an apparatus for preparing a solid product of tetra sodium hydroxyethylidene diphosphate of the present invention;

FIG. 2 is an enlarged schematic structural view of the tubular mixing reactor of the present invention;

in the drawings: 1, an HEDP aqueous solution storage tank, 2, a sodium hydroxide solution storage tank, 3, a tubular mixing reactor, 4, a tubular mixing reactor mounting bracket, 31, a tubular reaction section, 32, a tubular reaction section joint section, 33, a tubular reactant spraying section, 5, a granulation spray head, 311, an inwards concave annular groove with an arc-shaped vertical section, 6, an HEDP material liquid pump, 7, an HEDP aqueous solution conveying pipeline, 321, an HEDP aqueous solution input port, 8, an HEDP aqueous solution filter, 9, an HEDP aqueous solution flow meter, 10, an HEDP aqueous solution backflow pipeline, 11, an A electromagnetic valve, 12, a sodium hydroxide solution material liquid pump, 13, a sodium hydroxide solution conveying pipeline, 322, a sodium hydroxide solution input port, 14, a sodium hydroxide solution filter, 15, a sodium hydroxide solution flow meter, 16, a sodium hydroxide solution backflow pipeline, 17, a B electromagnetic valve, 18, cleaning water storage tank, 19, cleaning water pump, water pump, 20. The system comprises a cleaning water conveying pipeline, 323, a cleaning water conveying pipeline connecting port, 21, a cleaning water backflow pipeline, 22, a C electromagnetic valve, 23, a drying tower, 24, a fan, 25, an air suction pipeline, 26, a heat exchanger, 27, a hot air conveying pipe, 28, a dust remover and 29, and a star-shaped discharging device.

Detailed Description

The utility model discloses a concrete implementation mode is:

in the case of the example 1, the following examples are given,

as shown in fig. 1 and fig. 2, a preparation device of a solid product of hydroxyethylidene tetrasodium diphosphate is characterized in that: the device comprises an HEDP aqueous solution storage tank 1, an HEDP aqueous solution conveying device, a sodium hydroxide solution storage tank 2, a sodium hydroxide solution conveying device, an HEDP aqueous solution and sodium hydroxide solution mixed reaction device, a feeding liquid drying device for a reaction product of a solid target product of the hydroxyl ethylidene diphosphate tetrasodium obtained after the reaction of the HEDP and the sodium hydroxide is completed, a cleaning device for the HEDP aqueous solution and sodium hydroxide solution mixed reaction device and a control device;

the HEDP aqueous solution and sodium hydroxide solution mixed reaction device comprises a tubular mixed reactor 3 and a tubular mixed reactor mounting bracket 4, wherein the tubular mixed reactor mounting bracket 4 is arranged at the middle position of a steel-concrete platform, the tubular mixed reactor 3 is arranged on the top surface of the tubular mixed reactor mounting bracket 4, the tubular mixed reactor 3 arranged on the top surface of the tubular mixed reactor mounting bracket 4 is provided with a tubular reaction section 31, a tubular reaction section joint section 32 and a tubular reactant spraying section 33, the tubular reactant spraying section 33 is L-shaped, a granulation spray head 5 is arranged on the end part of the vertical part of the L-shaped tubular reactant spraying section in a threaded manner, and two ends of the tubular reaction section 31 of the tubular mixed reactor 3 are fixedly connected by using flanges and the end parts of the tubular reaction section joint section 32 and the end part of the transverse part of the tubular reactant spraying section 33 respectively; the middle section of a tubular reaction section 31 of the tubular mixed reactor 3 is a part with a thickened inner wall, the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is sequentially provided with 3 inward concave ring grooves 311 with arc vertical sections, the left notch of the leftmost vertical section of the inward concave ring groove 311 on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is connected with the arc surface of the left inner wall of the tubular reaction section 31 which is integrally formed, the right notch of the rightmost vertical section of the inward concave ring groove 311 on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is connected with the arc surface of the right inner wall of the tubular reaction section 31 which is integrally formed (an observer faces to the utility model, the left side of the observer is the leftmost vertical section of the inward concave ring groove, the right side of the observer is the rightmost vertical section of the inward concave ring groove), and; the length of the tubular reaction section 31 of the tubular mixed reactor 3 is 6 meters, and the inner diameter of the parts at two sides of the thickened middle section of the inner wall of the tubular reaction section 31 is 4.5 mm;

the HEDP aqueous solution conveying device comprises an HEDP aqueous solution pump 6 and an HEDP aqueous solution conveying pipeline 7, wherein the HEDP aqueous solution conveying pipeline 7 is provided with a vertical part and a horizontal part which are integrally formed, the end part of the vertical part of the HEDP aqueous solution conveying pipeline 7 is communicated, sealed and fixedly connected with an HEDP aqueous solution storage tank 1, the end part of the horizontal part is communicated, sealed and fixedly connected with an HEDP aqueous solution input port 321 arranged on a tubular reaction section joint section 32 arranged on a tubular mixing reactor 3, an HEDP aqueous solution filter 8 is arranged on the part, close to the HEDP aqueous solution storage tank 1, of the vertical part of the HEDP aqueous solution conveying pipeline 7 on the upper side of the HEDP aqueous solution filter 8, the HEDP aqueous solution pump 6 is arranged on the vertical part of the HEDP aqueous solution conveying pipeline 7 on the upper side of the HEDP aqueous solution pump 6, and an HEDP aqueous solution flowmeter 9 is arranged on the vertical part of the HEDP aqueous solution conveying pipeline 7 on the upper side of the HEDP aqueous solution pump 6; the HEDP water solution backflow pipeline 10 is provided with a vertical part and a horizontal part which are integrally formed, the end part of the vertical part of the HEDP water solution backflow pipeline 10 is communicated, sealed and fixedly connected with the HEDP water solution storage tank 1, the end part of the horizontal part is communicated, sealed and fixedly connected with a pipeline section part of the vertical part of an HEDP water solution conveying pipeline 7 between an HEDP water solution flowmeter 9 and an HEDP material liquid pump 6, and an A electromagnetic valve 11 is arranged on the horizontal part of the HEDP water solution backflow pipeline 10;

the sodium hydroxide solution conveying device comprises a sodium hydroxide solution feed liquid pump 12 and a sodium hydroxide solution conveying pipeline 13, wherein the sodium hydroxide solution conveying pipeline 13 is provided with a vertical part and a horizontal part which are integrally formed, the end part of the vertical part of the sodium hydroxide solution conveying pipeline 13 is communicated, sealed and fixedly connected with a sodium hydroxide solution storage tank 2, the end part of the horizontal part is communicated, sealed and fixedly connected with a sodium hydroxide solution inlet 322 arranged on a tubular reaction section joint section 32 of a tubular mixing reactor 3, a sodium hydroxide solution filter 14 is arranged on the part, close to the sodium hydroxide solution storage tank 2, of the vertical part of the sodium hydroxide solution conveying pipeline 13, the sodium hydroxide solution feed liquid pump 12 is arranged on the vertical part of the sodium hydroxide solution conveying pipeline 13 on the upper side of the sodium hydroxide solution pump 12, and a sodium hydroxide solution flowmeter 15 is arranged on the vertical part of the sodium hydroxide solution conveying pipeline 13 on the upper side of the sodium hydroxide solution feed liquid pump 12 (ii) a The system also comprises a sodium hydroxide solution return pipeline 16, wherein the sodium hydroxide solution return pipeline 16 is provided with a vertical part and a horizontal part which are integrally formed, the end part of the vertical part of the sodium hydroxide solution return pipeline 16 is communicated, sealed and fixedly connected with the sodium hydroxide solution storage tank 2, the end part of the horizontal part is communicated, sealed and fixedly connected with the pipeline section part of the vertical part of the sodium hydroxide solution conveying pipeline 13 between the sodium hydroxide solution flowmeter 15 and the sodium hydroxide solution liquid pump 12, and the horizontal part of the sodium hydroxide solution return pipeline 16 is provided with a B electromagnetic valve 17;

the cleaning device of the HEDP water solution and sodium hydroxide solution mixed reaction device comprises a cleaning water storage tank 18, a cleaning water pump 19 and a cleaning water pipeline 20, wherein the cleaning water pipeline 20 is provided with a vertical part and a horizontal part which are integrally formed, the end part of the vertical part of the cleaning water pipeline 20 is communicated, sealed and fixedly connected with the cleaning water storage tank 18, the end part of the horizontal part is communicated, sealed and fixedly connected with a cleaning water pipeline connecting port 323 arranged on a tubular reaction section joint section 32 of a tubular mixed reactor 3, the cleaning water pump 19 is arranged on the part, close to the cleaning water storage tank 18, of the vertical part of the cleaning water pipeline, and a cleaning water backflow pipeline 21, the cleaning water backflow pipeline 21 is provided with the vertical part and the horizontal part which are integrally formed, the end part of the vertical part of the cleaning water backflow pipeline 21 is communicated, sealed and fixedly connected with the cleaning water storage tank 18, the end part of the horizontal part is communicated with the vertical part of the pipeline section of the washing water delivery pipeline 20 on the upper side of the washing water pump 19 in a sealing and fixed way, and the horizontal part of the washing water backflow pipeline 21 is provided with a C electromagnetic valve 22;

the feed liquid drying device for the reaction product of the hydroxyethylidene tetrasodium diphosphate solid target product obtained after the reaction of HEDP and sodium hydroxide comprises a drying tower 23, a fan 24, an air suction pipeline 25, a heat exchanger 26 and a hot air conveying pipe 27, wherein the drying tower 23 is installed on a steel-concrete platform on the right side of a tubular mixed reactor installing support 4 by using a drying tower base, the part of a tubular reaction section of the tubular mixed reactor 3 installed on the top surface of the tubular mixed reactor installing support 4 and a tubular reactant spraying section provided with a granulating nozzle 5 and arranged on the tubular mixed reactor 3 penetrate through holes formed in the upper left side of the drying tower 23, extend into the drying tower 23, are fixedly installed on through holes formed in the upper left side of the drying tower 23 in a sealing manner, and extend into the drying tower 23 and are fixedly installed on the part of the tubular mixed reactor 3 reaction section on the through holes in the upper left side of the drying tower 23 in a sealing manner and the vertical axis of the granulating nozzle 5 of the tubular reactant spraying section 33 provided with the granulating nozzle and the drying tower 23 The vertical axis of the tower 23 is a straight line; the heat exchanger 26 is arranged on a steel-concrete platform at the lower part of the right side of the drying tower 23 by using a heat exchanger mounting seat, and a hot air delivery pipe 27 arranged on the heat exchanger 26 is fixedly connected with the lower part of the right side wall of the drying tower 23 in a penetrating and sealing manner; the air draft pipeline 25 is fixedly connected with the upper end part of the right side wall of the drying tower 23 in a penetrating and sealing way, the right end part of the air draft pipeline 25 is provided with a fan 24, and an air exhaust pipe is arranged on an air exhaust port of the fan 24; a dust remover 28 is also arranged on the air suction pipeline 25 on the left side of the fan 24; the inner surface of the bottom of the drying tower 23 is an inclined plane inclined towards the left side, a discharge hole is arranged at the position, close to the inner surface of the inclined plane inclined towards the left side, of the bottom of the left side of the bottom of the drying tower 23, and a star-shaped discharger 29 is mounted at the discharge hole arranged at the bottom of the left side of the bottom of the drying tower 23 through a mounting seat.

Use the utility model discloses the preparation equipment of the solid product of four sodium hydroxide ethylidene diphosphate prepares a solid product process of four sodium hydroxide ethylidene diphosphate is:

the solid product of the hydroxyl ethylidene diphosphate tetrasodium is prepared by reacting an HEDP aqueous solution with a sodium hydroxide solution, wherein the molar ratio of the HEDP to the sodium hydroxide is 1: 4.03; the preparation process of the solid product of the hydroxyl ethylidene diphosphate tetrasodium comprises the following steps:

A. according to the molar ratio of HEDP to sodium hydroxide reaction of 1: 4.03 preparing an aqueous HEDP solution and a sodium hydroxide solution correspondingly, wherein the volume ratio of the aqueous HEDP solution to the sodium hydroxide solution prepared correspondingly is 1: 0.79, the concentration of the HEDP aqueous solution is 60 percent (weight percentage), and the concentration of the sodium hydroxide solution is 40 percent (weight percentage); the HEDP aqueous solution and the sodium hydroxide solution which are prepared correspondingly are filled into an HEDP aqueous solution storage tank 1 and a sodium hydroxide solution storage tank 2 for standby;

B. starting the heat exchanger 26, wherein the temperature of hot air output by a hot air delivery pipe 27 arranged on the heat exchanger 26 is 55 ℃; starting the fan 24, and rising hot air output by the hot air delivery pipe 27 with the temperature of 55 ℃ along the drying tower 23;

C. starting the HEDP feed liquid pump 6, filtering the HEDP aqueous solution by an HEDP aqueous solution filter 8, metering the HEDP aqueous solution by an HEDP aqueous solution flowmeter 9, and conveying the HEDP aqueous solution to the tubular reaction section joint section 32 of the tubular mixing reactor 3 along the HEDP aqueous solution conveying pipeline 7 and through an HEDP aqueous solution input port 321 on the tubular reaction section joint section 32 which is fixedly connected with the HEDP aqueous solution conveying pipeline 7 in a penetrating and sealing manner through the transverse part end part; simultaneously starting a sodium hydroxide solution feed pump 12, filtering the sodium hydroxide solution by a sodium hydroxide solution filter 14, metering the sodium hydroxide solution by a sodium hydroxide solution flowmeter 15, and conveying the sodium hydroxide solution to a tubular reaction section joint section 32 of the tubular mixing reactor 3 through a sodium hydroxide solution input port 322 on a tubular reaction section joint section 32 which is fixedly connected with the sodium hydroxide solution conveying pipeline 13 in a sealing and penetrating way through the transverse part end part of the sodium hydroxide solution conveying pipeline 13; HEDP aqueous solution and sodium hydroxide solution which are simultaneously conveyed to a tubular reaction section joint section 32 of a tubular mixing reactor 3 are mixed and enter a tubular reaction section 31 of the tubular mixing reactor 3, HEDP entering the tubular reaction section 31 of the tubular mixing reactor and sodium hydroxide are reacted to obtain reaction product feed liquid of a solid target product of hydroxyethylidene diphosphonate, the reaction product feed liquid enters a tubular reactant spraying section 33 provided with a granulating nozzle 5 and is sprayed out by the granulating nozzle 5 to atomize the reaction product feed liquid of the solid target product of the hydroxyethylidene diphosphonate, the reaction of HEDP entering the tubular reaction section 31 of the tubular mixing reactor and sodium hydroxide belongs to exothermic reaction, the temperature of the reaction product feed liquid of the solid target product of the hydroxyethylidene diphosphonate sprayed out by the granulating nozzle 5 from the tubular reactant spraying section 33 provided with the granulating nozzle 5 is 115 ℃, and the temperature of the reaction product feed liquid of the solid target product of the hydroxyethylidene diphosphonate sprayed out by the granulating nozzle 5 from the tubular reactant spraying section 33 provided with the granulating nozzle 5 and the granulating nozzle 5 is controlled by the tubular reactant spraying section 33 provided with the granulating nozzle 5 The liquid of the reaction product of the sodium solid target product is in contact with the rising hot air at 55 ℃ in the drying tower 23 due to the gravity reduction, the moisture is vaporized and enters the gas phase, the hydroxyl ethylidene tetrasodium diphosphate solid powder finished product is obtained by drying, the hydroxyl ethylidene tetrasodium diphosphate solid powder falls to the bottom of the drying tower 23 and slides to a discharge port along the inclined inner surface of the bottom of the drying tower 23 which inclines leftwards, the hydroxyl ethylidene tetrasodium diphosphate solid powder is pulled out by a star-shaped discharge device 29 and enters the next processing procedure, and the waste gas in the drying tower 23 is dedusted by a deduster 28 and then is discharged by an exhaust pipe after reaching the standard;

D. and (3) equipment shutdown procedures: sequentially shutting down the HEDP material liquid pump 6 and the sodium hydroxide solution material liquid pump 12 in sequence, starting the cleaning water pump 19, conveying cleaning water to the tubular mixing reactor 3 along the cleaning water conveying pipeline 20, and sequentially cleaning the tubular reaction section joint section 32, the tubular reaction section 31 and the tubular reactant spraying section 33 provided with the granulation nozzle 5 of the tubular mixing reactor 3 for 10 seconds; sequentially shutting down the heat exchanger 23, the dust remover 28 and the fan 24 firstly and then, and shutting down the equipment;

the temperature of the HEDP aqueous solution is 25 ℃, and the temperature of the sodium hydroxide solution is 25 ℃;

the reaction pressure of the mixed reactor is 0.3MPa, and the reaction time is 3S;

the pump outlet pressure of the HEDP feed liquid pump and the pump outlet pressure of the sodium hydroxide solution feed liquid pump are both 0.42 MPa.

In the case of the example 2, the following examples are given,

the HEDP aqueous solution and sodium hydroxide solution mixed reaction device comprises a tubular mixed reactor 3 and a tubular mixed reactor mounting bracket 4, wherein the tubular mixed reactor mounting bracket 4 is arranged at the middle position of a steel-concrete platform, the tubular mixed reactor 3 is arranged on the top surface of the tubular mixed reactor mounting bracket 4, the tubular mixed reactor 3 arranged on the top surface of the tubular mixed reactor mounting bracket 4 is provided with a tubular reaction section 31, a tubular reaction section joint section 32 and a tubular reactant spraying section 33, the tubular reactant spraying section 33 is L-shaped, a granulation spray head 5 is arranged on the end part of the vertical part of the L-shaped tubular reactant spraying section in a threaded manner, and two ends of the tubular reaction section 31 of the tubular mixed reactor 3 are fixedly connected by using flanges and the end parts of the tubular reaction section joint section 32 and the end part of the transverse part of the tubular reactant spraying section 33 respectively; the middle section of a tubular reaction section 31 of the tubular mixed reactor 3 is a part with a thickened inner wall, the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is sequentially provided with 3 inward concave ring grooves 311 with arc vertical sections, the left notch of the leftmost vertical section of the inward concave ring groove 311 on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is connected with the arc surface of the left inner wall of the tubular reaction section 31 which is integrally formed, the right notch of the rightmost vertical section of the inward concave ring groove 311 on the inner surface of the thickened inner wall part of the middle section of the tubular reaction section is connected with the arc surface of the right inner wall of the tubular reaction section 31 which is integrally formed (an observer faces to the utility model, the left side of the observer is the leftmost vertical section of the inward concave ring groove, the right side of the observer is the rightmost vertical section of the inward concave ring groove), and the thickened inner wall of the middle section of the tubular reaction section is 0.5 mm; the length of the tubular reaction section 31 of the tubular mixed reactor 3 is 6.5 meters, and the inner diameter of the parts at two sides of the thickened middle section of the inner wall of the tubular reaction section 31 is 5 mm;

Use the utility model discloses the preparation equipment of the solid product of four sodium hydroxide ethylidene diphosphate prepares a solid product process of four sodium hydroxide ethylidene diphosphate is: the solid product of the hydroxyl ethylidene diphosphate tetrasodium is prepared by reacting an HEDP aqueous solution with a sodium hydroxide solution, wherein the molar ratio of the HEDP to the sodium hydroxide is 1: 4.08 of; the preparation process of the solid product of the hydroxyl ethylidene diphosphate tetrasodium comprises the following steps:

A. according to the molar ratio of HEDP to sodium hydroxide reaction of 1: 4.08 preparing HEDP aqueous solution and sodium hydroxide solution correspondingly, wherein the volume ratio of the HEDP aqueous solution to the sodium hydroxide solution prepared correspondingly is 1: 0.81, the concentration of the HEDP aqueous solution is 60 percent (weight percentage), and the concentration of the sodium hydroxide solution is 40 percent (weight percentage); the HEDP aqueous solution and the sodium hydroxide solution which are prepared correspondingly are filled into an HEDP aqueous solution storage tank 1 and a sodium hydroxide solution storage tank 2 for standby;

B. starting the heat exchanger 26, wherein the temperature of hot air output by a hot air delivery pipe 27 arranged on the heat exchanger 26 is 60 ℃; starting the fan 24, and rising hot air output by the hot air delivery pipe 27 with the temperature of 60 ℃ along the drying tower 23;

C. starting the HEDP feed liquid pump 6, filtering the HEDP aqueous solution by an HEDP aqueous solution filter 8, metering the HEDP aqueous solution by an HEDP aqueous solution flowmeter 9, and conveying the HEDP aqueous solution to the tubular reaction section joint section 32 of the tubular mixing reactor 3 along the HEDP aqueous solution conveying pipeline 7 and through an HEDP aqueous solution input port 321 on the tubular reaction section joint section 32 which is fixedly connected with the HEDP aqueous solution conveying pipeline 7 in a penetrating and sealing manner through the transverse part end part; simultaneously starting a sodium hydroxide solution feed pump 12, filtering the sodium hydroxide solution by a sodium hydroxide solution filter 14, metering the sodium hydroxide solution by a sodium hydroxide solution flowmeter 15, and conveying the sodium hydroxide solution to a tubular reaction section joint section 32 of the tubular mixing reactor 3 through a sodium hydroxide solution input port 322 on a tubular reaction section joint section 32 which is fixedly connected with the sodium hydroxide solution conveying pipeline 13 in a sealing and penetrating way through the transverse part end part of the sodium hydroxide solution conveying pipeline 13; HEDP aqueous solution and sodium hydroxide solution which are simultaneously conveyed to a tubular reaction section joint section 32 of the tubular mixing reactor 3 are mixed and enter a tubular reaction section 31 of the tubular mixing reactor 3, HEDP entering the tubular reaction section 31 of the tubular mixing reactor and sodium hydroxide are reacted to obtain reaction product feed liquid of a solid target product of hydroxyethylidene diphosphonate, the reaction product feed liquid enters a tubular reactant spraying section 33 provided with a granulation nozzle 5 and is sprayed out by the granulation nozzle 5 to atomize the reaction product feed liquid of the solid target product of the hydroxyethylidene diphosphonate, the reaction of HEDP entering the tubular reaction section 31 of the tubular mixing reactor and sodium hydroxide belongs to exothermic reaction, the temperature of the reaction product feed liquid of the solid target product of the hydroxyethylidene diphosphonate sprayed out by the granulation nozzle 5 from the tubular reactant spraying section 33 provided with the granulation nozzle 5 is 130 ℃, and the temperature of the reaction product feed liquid of the atomized tetra sodium hydroxyethylidene diphosphonate sprayed out by the tubular reactant spraying section 33 provided with the granulation nozzle 5 and the granulation nozzle 5 is controlled by the granulation nozzle 5 The liquid of the reaction product of the sodium solid target product is in contact with 60 ℃ hot air rising in the drying tower 23 due to gravity reduction, moisture is vaporized to enter a gas phase, and is dried to obtain a finished product of hydroxyl ethylidene tetrasodium diphosphate solid powder, the hydroxyl ethylidene tetrasodium diphosphate solid powder falls to the bottom of the drying tower 23 and slides to a discharge port along the inclined inner surface of the bottom of the drying tower 23, the inclined inner surface inclines leftwards, and is pulled out by a star-shaped discharge device 29 to enter the next processing procedure, and waste gas in the drying tower 23 is dedusted by a deduster 28 and then is discharged by an exhaust pipe to reach the standard;

D. and (3) equipment shutdown procedures: sequentially shutting down the HEDP material liquid pump 6 and the sodium hydroxide solution material liquid pump 12 firstly and secondly, starting a cleaning water pump 19, conveying cleaning water to the tubular mixing reactor 3 along a cleaning water conveying pipeline 20, and sequentially cleaning a tubular reaction section joint section 32, a tubular reaction section 31 and a tubular reactant spraying section 33 provided with a granulation nozzle 5 of the tubular mixing reactor 3 for 15 seconds; sequentially shutting down the heat exchanger 23, the dust remover 28 and the fan 24 firstly and then, and shutting down the equipment;

the temperature of the HEDP aqueous solution is 30 ℃, and the temperature of the sodium hydroxide solution is 30 ℃;

the reaction pressure of the mixed reactor is 0.5MPa, and the reaction time is 5S;

the outlet pressure of the HEDP feed liquid pump and the outlet pressure of the sodium hydroxide solution feed liquid pump are both 0.45 MPa.

The protection scope of the present invention is not limited to the scope described in the above embodiments, and all technical modifications made according to the principle of the present invention belong to the protection scope of the present invention.

Claims

1.A preparation device of a solid product of hydroxyl ethylidene diphosphate tetrasodium, which is characterized in that: the device comprises an HEDP aqueous solution storage tank, an HEDP aqueous solution conveying device, a sodium hydroxide solution storage tank, a sodium hydroxide solution conveying device, an HEDP aqueous solution and sodium hydroxide solution mixed reaction device, a device for drying feed liquid of a reaction product of a solid target product of the hydroxyl ethylidene diphosphate tetrasodium obtained after the reaction of the HEDP and the sodium hydroxide is completed, a cleaning device of the HEDP aqueous solution and sodium hydroxide solution mixed reaction device and a control device;

the sodium hydroxide solution conveying device comprises a sodium hydroxide solution feed pump, the device comprises a sodium hydroxide solution conveying pipeline, a sodium hydroxide solution conveying pipeline and a liquid level meter, wherein the sodium hydroxide solution conveying pipeline is provided with a vertical part and a horizontal part which are integrally formed, the end part of the vertical part of the sodium hydroxide solution conveying pipeline is communicated, sealed and fixedly connected with a sodium hydroxide solution storage tank, the end part of the horizontal part is communicated, sealed and fixedly connected with a sodium hydroxide solution inlet arranged on a tubular reaction section joint section of a tubular mixing reactor, a sodium hydroxide solution filter is arranged on the part, close to the sodium hydroxide solution storage tank, of the vertical part of the sodium hydroxide solution conveying pipeline, a sodium hydroxide solution liquid pump is arranged on the vertical part of the sodium hydroxide solution conveying pipeline on the upper side of the sodium hydroxide solution filter, and a sodium hydroxide solution flow meter is arranged on the vertical part of the sodium hydroxide solution conveying pipeline on the upper side of the sodium hydroxide solution liquid pump; the system also comprises a sodium hydroxide solution backflow pipeline, wherein the sodium hydroxide solution backflow pipeline is provided with a vertical part and a transverse part which are integrally formed, the end part of the vertical part of the sodium hydroxide solution backflow pipeline is communicated, sealed and fixedly connected with a sodium hydroxide solution storage tank, the end part of the transverse part is communicated, sealed and fixedly connected with a pipeline section part of the vertical part of a sodium hydroxide solution conveying pipeline between a sodium hydroxide solution flowmeter and a sodium hydroxide solution feed liquid pump, and a B electromagnetic valve is arranged on the transverse part of the sodium hydroxide solution backflow pipeline;

the cleaning device of the HEDP water solution and sodium hydroxide solution mixed reaction device comprises a cleaning water storage tank, a cleaning water pump and a cleaning water pipeline, wherein the cleaning water pipeline is provided with an integrally formed vertical part and a horizontal part, the end part of the vertical part of the cleaning water pipeline is communicated, sealed and fixedly connected with the cleaning water storage tank, the end part of the horizontal part is communicated, sealed and fixedly connected with a cleaning water pipeline connecting port arranged on a tubular reaction section joint section of the tubular mixed reactor, the cleaning water pump is arranged on the part, close to the cleaning water storage tank, of the vertical part of the cleaning water pipeline, the cleaning water reflux pipeline is provided with an integrally formed vertical part and a horizontal part, the end part of the vertical part of the cleaning water reflux pipeline is communicated, sealed and fixedly connected with the cleaning water storage tank, and the end part of the horizontal part is communicated, sealed and fixedly connected with the pipeline section of the vertical part of the cleaning water pipeline on the upper side of the cleaning water pump, the transverse part of the cleaning water backflow pipeline is provided with a C electromagnetic valve; the feed liquid drying device for the reaction product of the hydroxyethylidene tetrasodium diphosphate solid target product obtained after the reaction of the HEDP and the sodium hydroxide is completed comprises a drying tower, a fan, an air suction pipeline, a heat exchanger and a hot air conveying pipe, the drying tower is arranged on a steel-concrete platform on the right side of the mounting bracket of the tubular mixing reactor by using a drying tower base, the part of the tubular reaction section of the tubular mixing reactor arranged on the top surface of the mounting bracket of the tubular mixing reactor and the tubular reactant spraying section of the tubular mixing reactor provided with a granulating nozzle penetrate through a through hole arranged on the upper part of the left side of the drying tower and extend into the drying tower and are fixedly arranged on the through hole arranged on the upper part of the left side of the drying tower in a sealing way, the vertical axis of the granulation nozzle of the reaction section of the tubular mixed reactor, the tubular reactant spraying section provided with the granulation nozzle, and the vertical axis of the drying tower extend into the drying tower and are fixedly arranged on the through hole at the upper part of the left side of the drying tower in a sealing way; the heat exchanger is arranged on a steel-concrete platform at the lower part of the right side of the drying tower by using a heat exchanger mounting seat, and a hot air conveying pipe arranged on the heat exchanger is communicated, sealed and fixedly connected with the lower part of the right side wall of the drying tower; the air suction pipeline is fixedly connected with the upper end part of the right side wall of the drying tower in a penetrating and sealing way, the right end part of the air suction pipeline is provided with a fan, and an air exhaust pipe is arranged on an air exhaust port of the fan; the air suction pipeline on the left side of the fan is also provided with a dust remover; the inner surface of the bottom of the drying tower is an inclined plane inclined towards the left side, a discharge port is arranged at the position, close to the inner surface of the inclined plane inclined towards the left side, of the bottom of the left side of the bottom of the drying tower, and a star-shaped discharger is mounted at the discharge port arranged at the bottom of the left side of the bottom of the drying tower through a mounting seat.