Calcium formate continuous production device and process

文档序号:1038162 发布日期:2020-10-30 浏览:12次 中文

阅读说明:本技术 一种甲酸钙连续生产装置及工艺 (Calcium formate continuous production device and process ) 是由 郭启文 阴启建 张勇 汪达军 张兆明 于 2020-08-20 设计创作,主要内容包括:本发明公开了一种甲酸钙连续生产装置及工艺,属于甲酸钙生产技术领域,生产装置包括第一反应器、第二反应器、第三反应器,所述第一反应器的底部通过第一连通管与第二反应器的底部连通,第二反应器的上部通过第二连通管连通至第三反应器的中下部,第三反应器的底部通过管道连通至离心机的进料口,第三反应器的上部通过第一溢流口连通至杂质分离设备的上部。本发明提供的甲酸钙连续生产装置及工艺,采取第一反应器和第二反应器底部串联输送物料,第三反应器上部和底部分别出料的多级连续化反应方式,充分延长了反应时间,反应彻底充分,生产效率高,产品质量好,降低了生产成本和劳动强度,易于实现大规模连续化生产,适于广泛推广应用。(The invention discloses a continuous calcium formate production device and a continuous calcium formate production process, and belongs to the technical field of calcium formate production. According to the calcium formate continuous production device and the calcium formate continuous production process, a multistage continuous reaction mode that materials are conveyed in series at the bottoms of the first reactor and the second reactor and are discharged from the upper part and the bottom of the third reactor respectively is adopted, so that the reaction time is fully prolonged, the reaction is thorough and sufficient, the production efficiency is high, the product quality is good, the production cost and the labor intensity are reduced, large-scale continuous production is easy to realize, and the calcium formate continuous production device and the calcium formate continuous production process are suitable for wide popularization and application.)

1. A calcium formate continuous production device is characterized by comprising a first reactor, a second reactor, a third reactor, impurity separation equipment, a filter press, an evaporator, a centrifugal machine and a mother liquor tank;

the bottom of the first reactor is communicated to the bottom of the second reactor through a first communicating pipe, the upper part of the second reactor is communicated to the middle-lower part of the third reactor through a second communicating pipe, the bottom of the third reactor is communicated to a feed inlet of a centrifugal machine through a pipeline, and the upper part of the third reactor is communicated to the upper part of the impurity separation equipment through a first overflow port;

the upper part of the impurity separation equipment is also communicated to a feed inlet of the filter press through a second overflow port, and the bottom of the impurity separation equipment is communicated with the third reactor;

a liquid outlet of the centrifugal machine is communicated to a mother liquid tank through a pipeline;

the liquid outlet of the filter press is communicated to the liquid inlet of the evaporator and/or the mother liquid tank through a pipeline, and the liquid outlet of the evaporator is communicated to the second reactor through a pipeline;

the mother liquor tank is also communicated to the first reactor and/or the second reactor and/or the third reactor through a pipeline.

2. The continuous production device of calcium formate according to claim 1, wherein the impurity separator comprises a housing, wherein a first baffle plate and a second baffle plate are vertically and alternately arranged in the housing, the left and right sides of the first baffle plate and the second baffle plate are fixedly connected with the side wall of the housing, and the bottom edges of the first baffle plate and the second baffle plate are spaced from the bottom wall of the housing;

the baffling mouth has all been seted up at the top of first baffling board and second baffling board, and the baffling mouth on the first baffling board sets up with the baffling mouth is crisscross on the second baffling board, and the position of second overflow mouth is less than the position of first overflow mouth, and the position of first overflow mouth is less than the top of first baffling board and second baffling board.

3. The continuous calcium formate production apparatus of claim 2, wherein the bottom wall of the casing is inclined downward toward the third reactor.

4. The continuous production device of calcium formate according to claim 2, wherein the lower portion of the housing is provided with a water inlet and a flushing outlet, the water inlet is communicated with the mother liquor under a certain pressure, and the flushing outlet is communicated with the bottom of the third reactor.

5. The continuous calcium formate production device as claimed in claim 1, wherein the liquid outlet of the evaporator is connected to the bottom of the second reactor via a pipeline, and the mother liquor tank is connected to the bottom of the first reactor and/or the second reactor and/or the third reactor via a pipeline.

6. The continuous calcium formate production device of claim 1, wherein heating coils are disposed in the first reactor, the second reactor and the third reactor, and stirrers are disposed in the first reactor, the second reactor, the third reactor and the mother liquor tank.

7. The continuous calcium formate production device as claimed in claim 1, further comprising a first buffer tank and/or a second buffer tank, wherein the upper part of the first buffer tank is communicated with a second overflow port on the impurity separation device through a pipeline, the lower part of the first buffer tank is communicated with a feed port of the filter press through a pipeline, the upper part of the second buffer tank is communicated with a drain port of the filter press through a pipeline, the lower part of the second buffer tank is communicated with a liquid inlet of the evaporator through a pipeline, and a stirrer is arranged in the first buffer tank and/or the second buffer tank.

8. The continuous production apparatus of calcium formate according to claim 1, wherein said centrifuge is a pusher centrifuge and said filter press is a membrane filter press.

9. A continuous production process of calcium formate is characterized in that a first reactor, a second reactor and a third reactor are adopted, a formic acid solution and calcium carbonate powder are continuously added into the first reactor and uniformly stirred to react, a reaction material at the bottom of the first reactor is pressed into the second reactor from the bottom of the second reactor through pressure, and a reaction material at the upper part of the second reactor overflows into the third reactor;

extracting a bottom reaction material from the bottom of the third reactor, separating the bottom reaction material to obtain a calcium formate crude product and a mother liquor, returning the mother liquor to the first reactor and/or the second reactor and/or the third reactor, and drying and sieving the calcium formate crude product to obtain a calcium formate product; overflowing the upper reaction material from the upper part of the third reactor, separating entrained water insoluble substances from the upper reaction material to obtain a liquid phase, mixing the liquid phase with the mother liquor, and returning the liquid phase to the first reactor and/or the second reactor and/or the third reactor, or evaporating and concentrating the liquid phase and returning the liquid phase to the second reactor.

10. The continuous production process of calcium formate according to claim 9, wherein the concentration of the formic acid solution is 85-95%, the purity of calcium carbonate is more than 95%, the weight ratio of the formic acid solution and calcium carbonate powder added to the first reactor is (1.03-1.15):1, the temperature of the materials in each reactor is 30-50 ℃, and the pH value in each reactor is 3.5-4.

Technical Field

The invention relates to a calcium formate continuous production device and a calcium formate continuous production process, and belongs to the technical field of calcium formate production.

Background

The main method for producing calcium formate is to react formic acid solution with calcium carbonate to produce calcium formate product solution, to remove insoluble substances in the product solution by filtration, to obtain filtrate, to concentrate, crystallize, centrifugally separate, and dry to obtain calcium formate product. The traditional calcium formate production process is an intermittent reaction, wherein a formic acid solution and calcium carbonate are slowly added into a reactor according to a reaction ratio, and are mixed with a mother solution added through stirring to fully react. And (3) stopping feeding after the volume of the reactor is fed to a proper liquid level, continuously reacting the reaction materials in the reactor for about 2.5 hours, analyzing the components of the reaction liquid to reach the standard, and conveying the product solution to a scraper centrifuge by a feeding pump. And conveying the centrifuged materials to a dryer, conveying the dried finished products to a storage bin through a scraper conveyor, and packaging according to specifications for sale.

The traditional production process of calcium formate has the following problems:

(1) in the traditional process, the time intervals of feeding, reacting and discharging exist in the production process, so that the reaction process cannot be continuously carried out, the time from feeding to the reaction kettle to stopping the reaction is about 4 hours, the time consumption is long, the output rate of equipment is low, the yield is low, and the energy consumption is high.

(2) The content of calcium formate water-insoluble substances is a core index of calcium formate products, and unclean impurity removal can influence the whiteness of the calcium formate products and is difficult to develop in the market. The water insoluble substance is mainly from impurities in the calcium carbonate raw material, and the impurities enter the reaction kettle along with the calcium carbonate and are aggregated, so that the calcium formate has poor crystallization effect and small crystal particle size. In the traditional process, in order to reduce the content of the water-insoluble substances, the product solution needs to be precipitated in a reaction kettle for about 0.5 hour to discharge the water-insoluble substances and impurities on the upper layer, so that the reaction cannot be continuously carried out, the consumed time is long, the calcium formate product is easily lost due to the discharge of the water-insoluble substances and the impurities, and the material waste is serious.

(3) The mother liquor is surplus due to water brought into the system in the formic acid and water of a reaction byproduct, in the traditional process, the mother liquor needs to be discharged intermittently according to the liquid level of the mother liquor, and the surplus water is discharged, so that the loss of a calcium formate product in the mother liquor is easily caused.

(4) In the traditional process, a centrifugal machine for separating calcium carbonate products needs to clean filter cloth regularly, generally, the filter cloth is cleaned once every 5 days, and each time needs about 4 hours, so that the capacity is severely restricted.

(5) The calcium formate obtained after centrifugation is dried in a drier, the generated water vapor enters a dust remover for treatment, and impurities contained in the calcium formate prepared in the traditional process are discharged along with air flow, so that the dust remover discharges more powder.

The above description is included in the technical recognition scope of the inventors, and does not necessarily constitute the prior art.

Disclosure of Invention

The invention aims to solve the problems in the prior art, and provides a calcium formate continuous production device and a calcium formate continuous production process, so that large-scale continuous production can be realized, the yield of calcium formate is increased, the labor intensity is reduced, and the production cost is reduced.

The invention adopts the following technical scheme to realize the purpose:

in one aspect, the invention provides a calcium formate continuous production device, which comprises a first reactor, a second reactor, a third reactor, impurity separation equipment, a filter press, an evaporator, a centrifugal machine and a mother liquor tank, wherein the first reactor is connected with the second reactor;

the bottom of the first reactor is communicated to the bottom of the second reactor through a first communicating pipe, the upper part of the second reactor is communicated to the middle-lower part of the third reactor through a second communicating pipe, the bottom of the third reactor is communicated to a feed inlet of a centrifugal machine through a pipeline, and the upper part of the third reactor is communicated to the upper part of the impurity separation equipment through a first overflow port;

the upper part of the impurity separation equipment is also communicated to a feed inlet of the filter press through a second overflow port, and the bottom of the impurity separation equipment is communicated with the third reactor;

a liquid outlet of the centrifugal machine is communicated to a mother liquid tank through a pipeline;

the liquid outlet of the filter press is communicated to the liquid inlet of the evaporator and/or the mother liquid tank through a pipeline, and the liquid outlet of the evaporator is communicated to the second reactor through a pipeline;

the mother liquor tank is also communicated to the first reactor and/or the second reactor and/or the third reactor through a pipeline.

Optionally, the impurity separation device includes a housing, wherein a first baffle plate and a second baffle plate are vertically and alternately arranged in the housing, left and right sides of the first baffle plate and the second baffle plate are fixedly connected to a side wall of the housing, and bottom edges of the first baffle plate and the second baffle plate have a certain interval with a bottom wall of the housing;

the baffling mouth has all been seted up at the top of first baffling board and second baffling board, and the baffling mouth on the first baffling board sets up with the baffling mouth is crisscross on the second baffling board, and the position of second overflow mouth is less than the position of first overflow mouth, and the position of first overflow mouth is less than the top of first baffling board and second baffling board.

Optionally, the bottom wall of the shell is arranged obliquely downwards towards the direction close to the third reactor.

Optionally, the lower part of the shell is provided with a water inlet and a flushing outlet, the water inlet is communicated with the mother liquor with a certain pressure, and the flushing outlet is communicated with the bottom of the third reactor.

Optionally, a liquid outlet of the evaporator is communicated to the bottom of the second reactor through a pipeline, and the mother liquor tank is communicated to the bottoms of the first reactor and/or the second reactor and/or the third reactor through a pipeline.

Optionally, heating coils are arranged in the first reactor, the second reactor and the third reactor, and stirrers are arranged in the first reactor, the second reactor, the third reactor and the mother liquor tank.

Optionally, the calcium formate continuous production device further comprises a first buffer tank and/or a second buffer tank, the upper portion of the first buffer tank is communicated with a second overflow port on the impurity separation device through a pipeline, the lower portion of the first buffer tank is communicated with a feed port of the filter press through a pipeline, the upper portion of the second buffer tank is communicated with a drain port of the filter press through a pipeline, the lower portion of the second buffer tank is communicated with a liquid inlet of the evaporator through a pipeline, and a stirrer is arranged in the first buffer tank and/or the second buffer tank.

Optionally, the centrifuge is a pusher centrifuge, and the filter press is a diaphragm filter press.

On the other hand, the invention also provides a calcium formate continuous production process, which adopts a first reactor, a second reactor and a third reactor, wherein a formic acid solution and calcium carbonate powder are continuously added into the first reactor and uniformly stirred for reaction, a reaction material at the bottom of the first reactor is pressed into the second reactor from the bottom of the second reactor through pressure, and a reaction material at the upper part of the second reactor overflows into the third reactor;

extracting a bottom reaction material from the bottom of the third reactor, separating the bottom reaction material to obtain a calcium formate crude product and a mother liquor, returning the mother liquor to the first reactor and/or the second reactor and/or the third reactor, and drying and sieving the calcium formate crude product to obtain a calcium formate product; overflowing the upper reaction material from the upper part of the third reactor, separating entrained water insoluble substances from the upper reaction material to obtain a liquid phase, mixing the liquid phase with the mother liquor, and returning the liquid phase to the first reactor and/or the second reactor and/or the third reactor, or evaporating and concentrating the liquid phase and returning the liquid phase to the second reactor.

Optionally, the concentration of the used formic acid solution is 85-95%, the purity of the calcium carbonate is more than 95%, and the weight ratio of the formic acid solution to the calcium carbonate powder added into the first reactor is (1.03-1.15) to 1, preferably 1.08: 1; the material temperature in each reactor is 30-50 ℃, preferably 40 ℃; the pH value in each reactor is 3.5-4.

The calcium formate continuous production device and the calcium formate continuous production process provided by the invention optimize the calcium formate production device and the calcium formate production process and have the following beneficial effects:

(1) the feeding ports and the discharging ports of the reactors are reasonably arranged, the multistage continuous reaction mode that materials are conveyed from the bottoms of the first reactor and the second reactor in series and discharged from the upper part and the bottom of the third reactor respectively is adopted, the reaction materials are conveyed from the first reactor to the second reactor by utilizing the self pressure of the reaction materials, the reaction materials are conveyed from bottom to top and overflow from the upper part to the third reactor after entering the second reactor, and finally are extracted from the bottom of the third reactor, so that the reaction time is fully prolonged, and the reaction is thorough and full;

(2) reasonably determining the volume of reaction materials in the reactor, the feeding speed of formic acid solution and calcium carbonate, the discharging speed of the reaction materials, the reaction temperature and the pH value according to the required reaction time, so that the circulation quantity of the reaction materials in the system is increased, the solid-liquid ratio bearable by the system is increased, the reaction is thorough and sufficient, and the prepared calcium formate product has uniform granularity;

(3) a part of liquid phase obtained by solid-liquid separation and filtration of the discharged material at the upper part of the third reactor can be discharged out of the surplus water in the system after evaporation concentration, so that water insoluble impurities are effectively separated, the product purity is improved, the liquid phase after evaporation concentration is returned to the second reactor with higher concentration for continuous crystallization, the calcium formate product in the discharged material at the upper part is effectively recovered, and the product yield is improved;

(4) the stirrer is arranged in the reactor to stir the reaction materials, so that the materials can be uniformly mixed and fully reacted, the problem that the reaction materials containing calcium formate are accumulated in the reactor or a pipeline is blocked due to poor fluidity can be avoided, and the reaction can be continuously carried out; the stirrer in the third reactor is only provided with stirring blades at the lower part, and only the reaction materials at the lower part are stirred and boosted, so that the influence of stirring the reaction materials at the upper part on the floating and overflowing effect of water-insoluble substances in the reaction materials at the upper part is avoided, and the product purity is improved;

(5) the mother liquor returns to each reactor through a pipeline to flush and boost the materials at the bottom of the reactor, so that the materials are smoothly circulated in the system, and the deposition and aggregation are prevented; especially, the mother liquor returned to the first reactor can also play a role in adjusting the solid-liquid ratio in the system material.

In conclusion, the calcium formate continuous production device and the calcium formate continuous production process provided by the invention have the advantages of simple overall process, high production efficiency and good product quality, reduce the production cost and labor intensity, are easy to realize large-scale continuous production, and are suitable for wide popularization and application.

Drawings

The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:

fig. 1 is a schematic structural diagram of a calcium formate continuous production apparatus provided in the present application;

FIG. 2 is a schematic structural diagram of an impurity separation apparatus in a calcium formate continuous production apparatus provided in the present application;

FIG. 3 is a left side view of FIG. 2;

fig. 4 is a schematic structural diagram of a first baffle plate and a second baffle plate in an impurity separation device in a continuous calcium formate production apparatus provided by the present invention;

fig. 5 is a schematic perspective view of a part of the structure of an impurity separation device in a calcium formate continuous production apparatus provided by the present invention;

FIG. 6 is a schematic layout diagram of an impurity separation device and a third reactor in a calcium formate continuous production apparatus provided by the present invention;

in the figure, 110, the first reactor; 120. a second reactor; 130. a third reactor; 140. a first communication pipe; 150. a second communicating pipe; 160. a first overflow port; 170. a second overflow port; 101. a heating coil; 102. a stirrer; 200. a centrifuge; 300. a mother liquor tank; 400. an impurity separation device; 410. a housing; 420. a first baffle plate; 430. a second baffle plate; 440. a baffling port; 450. a water inlet; 460. a flushing port; 500. a filter press; 600. an evaporator; 700. a dryer; 800. a first buffer tank; 900. a second buffer tank.

Detailed Description

The present invention will be described in further detail below with reference to the attached drawings. It should be noted, however, that the following detailed description merely gives specific operation examples of the present invention by way of example, and the scope of the present invention is not limited thereto. The scope of the invention is limited only by the claims. It will be obvious to those skilled in the art that various other modifications and substitutions can be made to the described embodiments of the invention within the scope of the invention as defined by the claims and still achieve the same technical result and achieve the final technical object of the invention.

As shown in fig. 1, in one aspect, the present invention provides a continuous calcium formate production apparatus, including a first reactor 110, a second reactor 120, a third reactor 130, an impurity separation device 400, a filter press 500, an evaporator 600, a centrifuge 200, and a mother liquor tank 300;

wherein, the bottom of the first reactor 110 is communicated to the bottom of the second reactor 120 through a first communicating pipe 140, the upper part of the second reactor 120 is communicated to the middle-lower part of the third reactor 130 through a second communicating pipe 150, the bottom of the third reactor 130 is communicated to the feed inlet of the centrifuge 200 through a pipeline, and the upper part of the third reactor 130 is communicated to the upper part of the impurity separating device 400 through a first overflow port 160;

the upper part of the impurity separation device 400 is also communicated to the feed inlet of the filter press 500 through a second overflow port 170, and the bottom of the impurity separation device 400 is communicated with the third reactor 130;

the liquid outlet of the centrifuge 200 is communicated to the mother liquid tank 300 through a pipeline;

the liquid outlet of the filter press 500 is communicated with the liquid inlet of the evaporator 600 and/or the mother liquid tank 300 through a pipeline, and the liquid outlet of the evaporator 600 is communicated with the second reactor 120 through a pipeline;

further, the installation positions of the first reactor 110, the second reactor 120 and the third reactor 130 are sequentially lowered, and the first communicating pipe 140 between the first reactor 110 and the second reactor 120 and the second communicating pipe 150 between the second reactor 120 and the third reactor 130 are downwardly inclined toward the downstream of the flowing direction of the reaction materials, so that the reaction materials can be smoothly and sequentially transferred between the reactors. The specific production process comprises the following steps: the formic acid solution and the calcium carbonate powder are added into the first reactor 110 to start reaction, the reaction materials in the first reactor 110 contain unreacted formic acid and calcium carbonate, calcium formate generated by the reaction, water carried by the formic acid solution and a reaction byproduct and impurities carried by the calcium carbonate powder, the reaction materials are pressed into the second reactor 120 from the bottom of the first reactor 110 by liquid level difference while continuing to react, and the reaction materials flow from bottom to top after entering the second reactor 120 and overflow from the upper part of the second reactor 120 to enter the third reactor 130. The chemical reaction in the third reactor 130 is substantially completed, the resulting high-concentration calcium formate material is accumulated at the bottom of the third reactor 130, and the water-insoluble impurities float at the upper part of the third reactor 130.

The bottom reaction material in the third reactor 130 is conveyed to the centrifuge 200 by a feeding pump of the centrifuge 200, the solid material obtained by centrifugation is a crude calcium formate product, and the centrifugate obtained by centrifugation enters the mother liquor tank 300 to be sent back to the reactor. The upper reaction material in the third reactor 130 overflows from the first overflow port 160 and enters the impurity separation device 400, part of water insoluble impurities in the upper reaction material are separated in the impurity separation device 400, collected and then enter the filter press 500, the impurities are removed by filter pressing of the filter press 500, part of the liquid phase obtained by the filter press 500 directly enters the mother liquid tank 300 for collection, and part of the liquid phase is evaporated by the evaporator 600 to remove the residual water and then is sent to the second reactor 120. It is understood that the mother liquor contains formic acid, water and a small amount of calcium formate.

In order to effectively separate the water-insoluble impurities from the mother liquor in the upper reaction material in the third reactor 130 and discharge the residual water in the upper reaction material, as shown in fig. 2-5, the impurity separation apparatus 400 provided by the present invention comprises a housing 410, wherein a first baffle plate 420 and a second baffle plate 430 are vertically and alternately arranged in the housing 410, the left and right sides of the first baffle plate 420 and the second baffle plate 430 are fixedly connected with the side wall of the housing 410, and the bottom sides of the first baffle plate 420 and the second baffle plate 430 are spaced from the bottom wall of the housing 410;

the baffling ports 440 are formed in the tops of the first baffling plate 420 and the second baffling plate 430, the baffling ports 440 on the first baffling plate 420 and the baffling ports 440 on the second baffling plate 430 are arranged in a staggered mode, the position of the second overflow port 170 is lower than that of the first overflow port 160, and the position of the first overflow port 160 is lower than that of the tops of the first baffling plate 420 and the second baffling plate 430.

The upper reaction material overflows into the casing 410 and then flows to the second overflow port 170 at a lower position, and in the flowing process, the calcium formate with high density gradually settles to the bottom of the casing 410, and the water-insoluble impurities with low density float to the upper part. The first baffle plate 420 and the second baffle plate 430 are arranged to enable the material to flow in an S shape on the upper portion of the shell 410, so that the flow time of the material is prolonged, and the separation effect is improved. The water-insoluble impurities with low density overflow from the second overflow port 170 and enter the filter press 500 for separation, and the obtained liquid phase enters the evaporator 600 to evaporate the rich residual water.

The number of the first baffle plate 420 and the second baffle plate 430 can be adjusted according to actual conditions. The number of the first and second baffle plates 420 and 430 shown in fig. 2 and 5 is 3 in total.

In the shell 410, the calcium formate may settle to the bottom of the shell 410, and in order to collect the calcium formate for easy cleaning and reduce dead space accumulation in the shell 410, in one embodiment, the bottom wall of the shell 410 is disposed obliquely downward toward the third reactor 130.

Further, in order to clean the calcium formate accumulated at the bottom of the shell 410, in another embodiment, a water inlet 450 and a flushing outlet 460 are opened at the lower part of the shell 410, the water inlet 450 is communicated with the mother liquor under a certain pressure, and the flushing outlet 460 is communicated with the bottom of the third reactor 130. During production, high-pressure jet flow mother liquor is introduced into the shell 410 through the water inlet 450, the mother liquor impacts the bottom of the shell 410, calcium formate is flushed up and discharged from the flushing outlet 460 to enter the third reactor 130, and then calcium formate crude products are obtained by centrifugal separation from the third reactor 130.

Generally, as shown in fig. 6, the shell 410 has an arc shape, the shell 410 is wrapped around the arc 1/4 of the third reactor 130, and the upper portion of the first reactor 110 is provided with a plurality of overflow ports to communicate with the shell 410.

The liquid outlet of the filter press 500 is communicated to the liquid inlet of the evaporator 600 and/or the mother liquid tank 300 through a pipeline, the water content of the liquid phase discharged by the filter press 500 is higher, one part of the liquid phase is directly collected in the mother liquid tank 300, the other part of the liquid phase is evaporated by the evaporator 600 to remove the surplus water and then is sent to the second reactor 120, and the mother liquid is evaporated and concentrated and then returns to the second reactor 120 with higher concentration to enable the calcium formate in the mother liquid to be crystallized continuously. The mother liquor returns to each reactor from the mother liquor tank 300 through a pipeline to flush and boost the materials in the reactors, so that the materials can smoothly circulate in the system, the deposition and aggregation are prevented, and especially the mother liquor returns to the first reactor 110 to play a role in adjusting the solid-to-liquid ratio of the materials in the system.

Further, a liquid outlet of the evaporator 600 is connected to the bottom of the second reactor 120 through a pipe, and the liquid phase enters the second reactor 120 from the bottom of the second reactor 120 after being concentrated. The mother liquor tank 300 is communicated to the bottom of the first reactor 110, the second reactor 120 and/or the third reactor 130 through a pipeline, and mother liquor enters the bottom of the reactors to perform intensive flushing on bottom materials in the reactors.

Further, heating coils 101 are disposed in the first reactor 110, the second reactor 120, and the third reactor 130, and a stirrer 102 is disposed in the first reactor 110, the second reactor 120, the third reactor 130, and the mother liquor tank 300.

Specifically, steam is introduced into the heating coil 101 to control the reaction temperature in the reactor.

The stirrer 102 is put into the reactor, so that the materials can be uniformly and fully mixed and react, the materials can be pushed to be conveyed, the defect that the system cannot smoothly produce due to high solid content is overcome, the materials are prevented from being deposited or blocked by a pipeline, the shutdown and cleaning are avoided, and the continuous production of feeding and discharging is realized. The stirrer 102 in the third reactor 130 is only provided with a stirring blade at the lower part to stir and boost the lower part reaction materials, and the stirring speed is not too high, so that the floating overflow effect of the water-insoluble substances in the upper part reaction materials is prevented from being influenced by stirring the upper part reaction materials, and the product purity is improved.

The stirrer 102 is arranged in the mother liquid tank 300, so that material accumulation and deposition can be prevented, the material can be returned to the reactor for recovery, the reaction can be promoted to be continuously carried out, and the difficulty in cleaning the mother liquid tank 300 is reduced.

In a preferred embodiment, the continuous calcium formate production apparatus provided by the present invention further includes a first buffer tank 800 and/or a second buffer tank 900, an upper portion of the first buffer tank 800 is communicated with the second overflow port of the impurity separation device 400 through a pipeline, a lower portion of the first buffer tank 800 is communicated with the feed port of the filter press 500 through a pipeline, an upper portion of the second buffer tank 900 is communicated with the drain port of the filter press 500 through a pipeline, a lower portion of the second buffer tank 900 is communicated with the liquid inlet of the evaporator 600 through a pipeline, and a stirrer 102 is disposed in the first buffer tank 800 and/or the second buffer tank 900 and is used for stirring materials in the tanks. The first buffer tank 800 is used to collect the clear liquid discharged from the impurity separating apparatus 400, and the second buffer tank 900 is used to collect the drain liquid of the filter press 500.

In another embodiment, the continuous calcium formate production apparatus provided by the present invention further includes a dryer 700, where the dryer 700 is used to dry calcium formate solids discharged from the centrifuge 200, a bottom reaction material in the third reactor 130 is conveyed to the centrifuge 200 through a feeding pump of the centrifuge 200, the centrifuged material is conveyed to the dryer 700, and a dried finished product is conveyed to a bin through a scraper and packaged according to specifications for sale.

The centrifuge 200 is preferably a pusher centrifuge 200, capable of continuous operation; the filter press 500 is preferably a membrane filter press 500 capable of efficiently separating water-insoluble impurities; the evaporator 600 is preferably an MVR evaporator 600.

On the other hand, the invention also provides a calcium formate continuous production process, which comprises the steps of adopting a first reactor 110, a second reactor 120 and a third reactor 130, continuously adding a formic acid solution and calcium carbonate powder into the first reactor 110, uniformly stirring and reacting, pressing a reaction material at the bottom of the first reactor 110 into the second reactor 120 from the bottom of the second reactor 120 through pressure, and overflowing the reaction material at the upper part of the second reactor 120 into the third reactor 130;

overflowing an upper reaction material from the upper part of the third reactor 130, extracting a bottom reaction material from the bottom of the third reactor 130, wherein the bottom reaction material mainly comprises calcium formate, formic acid and water, separating the bottom reaction material to obtain a crude calcium formate product and a mother liquor, and drying and sieving the crude calcium formate product to obtain a calcium formate product. The upper reaction materials mainly comprise formic acid, water, a small amount of calcium formate and floating water-insoluble impurities, a liquid phase is obtained after the water-insoluble impurities carried in the upper reaction materials are separated, a part of the liquid phase returns to the first reactor and/or the second reactor and/or the third reactor, and a part of the liquid phase returns to the second reactor after evaporation and concentration.

The number of reactors is not limited to three, and may be increased according to the flow principle of the reaction materials and the required reaction time and yield in the present invention.

Further, the concentration of the formic acid solution is 85-95%, the purity of calcium carbonate is more than 95%, and the weight ratio of the formic acid solution and calcium carbonate powder added into the first reactor 110 is (1.03-1.15) to 1, preferably 1.08: 1; the material temperature in each reactor is 30-50 ℃, preferably 40 ℃; the pH value in each reactor is 3.5-4.

In order to more clearly explain the overall concept of the present application, the following detailed description will be given by way of specific examples.

14页详细技术资料下载
上一篇:一种医用注射器针头装配设备
下一篇:一种甲基丙烯酸钠的连续化生产工艺及其设备

网友询问留言

已有0条留言

还没有人留言评论。精彩留言会获得点赞!

精彩留言,会给你点赞!