CN113548685A

CN113548685A - Preparation process and device for synthesizing nano calcium carbonate based on composite inducer

Info

Publication number: CN113548685A
Application number: CN202110683138.6A
Authority: CN
Inventors: 杨保俊; 王百年; 陈小龙; 王鑫
Original assignee: Hefei University of Technology
Current assignee: Hefei University of Technology
Priority date: 2021-06-21
Filing date: 2021-06-21
Publication date: 2021-10-26
Anticipated expiration: 2041-06-21
Also published as: CN113548685B

Abstract

The invention discloses a preparation process and a device for synthesizing nano calcium carbonate based on a composite inducer, which comprises the following steps: step 100: dissolving ammonium chloride powder into deionized water, adding carbide slag, and removing solid impurities in the reaction liquid to obtain carbide slag leaching liquid; step 200: placing the carbide slag leaching solution into a closed normal-pressure reaction kettle, adding a composite inducer, adjusting the temperature of the normal-pressure reaction kettle to a preset temperature, continuously introducing carbon dioxide, stirring the reaction solution in the normal-pressure reaction kettle for reaction in a closed state, and stopping introducing the carbon dioxide when the pH value reaches a preset value to finish a precipitation process; step 300: carrying out solid-liquid separation on the reaction solution after the precipitation process is finished; step 400: and washing and drying the obtained filter cake to obtain the nano calcium carbonate sample. The invention can maintain the relative stability of the pH value of the solution, so that the reaction is more complete and the product can approach the target form.

Description

Preparation process and device for synthesizing nano calcium carbonate based on composite inducer

Technical Field

The invention relates to the technical field of nano calcium carbonate, in particular to a preparation process and a device for synthesizing nano calcium carbonate based on a composite inducer.

Background

At present, relevant statistics show that the annual production of PVC by using calcium carbide as a raw material in China reaches 2400 ten thousand tons, and the annual production of calcium carbide slag is about 4300 ten thousand tons. At present, the accumulated stacking amount of the carbide slag in China exceeds billions of tons, and as the water filtrate of the carbide slag is strong in alkalinity (the pH value is more than 12), most enterprises adopt a sand burying or open stacking mode to dispose the carbide slag, so that the comprehensive utilization rate is low. The accumulation of a large amount of carbide slag not only occupies land resources, but also can salinize the land and pollute underground water, and meanwhile, toxic and harmful substances generated during the hydrolysis of the carbide seriously endanger the surrounding environment and the living health of residents. Therefore, comprehensive utilization of resources is urgently needed. Carbide slag contains rich Ca (OH)₂The method is widely applied to a plurality of industries such as building materials, chemical engineering and the like, wherein the chemical industry field is mainly used for preparing cement, propylene oxide, soda ash, potassium chlorate, calcium carbonate and the like. Comprehensively considering the existing utilization technology of the carbide slag, the preparation of the nano calcium carbonate from the carbide slag has excellent economic benefit.

In the prior art, the production reaction of calcium carbonate is generally completed in an open environment, but the temperature of the solution in the open environment is difficult to keep constant, and the change of the temperature of the solution can cause the solubility of carbon dioxide in the solution to change, thereby causing the pH value of the solution to change, and finally easily causing the product not to reach the target form, incomplete reaction and the like.

Disclosure of Invention

The invention aims to provide a preparation process and a device for synthesizing nano calcium carbonate based on a composite inducer, which aim to solve the technical problem that the preparation process for synthesizing the nano calcium carbonate with small particle size, uniform dispersion and narrow particle size distribution under higher initial concentration is urgently needed to be developed in the prior art.

In order to solve the technical problems, the invention specifically provides the following technical scheme:

a preparation process for synthesizing nano calcium carbonate based on a composite inducer comprises the following steps:

step 100: dissolving ammonium chloride powder into deionized water, adding carbide slag, and removing solid impurities in a reaction solution after completely reacting at room temperature to obtain a carbide slag leaching solution;

step 200: placing the carbide slag leaching solution into a closed normal-pressure reaction kettle, adding a composite inducer, adjusting the temperature of the normal-pressure reaction kettle to a preset temperature, continuously introducing carbon dioxide, stirring the reaction solution in the normal-pressure reaction kettle for reaction in a closed state, monitoring the pH value of the reaction solution in real time, and stopping introducing the carbon dioxide when the pH value reaches a preset value to finish a precipitation process;

step 300: carrying out solid-liquid separation on the reaction solution after the precipitation process is finished;

step 400: and washing and drying the obtained filter cake to obtain a nano calcium carbonate sample, wherein the obtained filtrate is an ammonium chloride solution and is circularly used for preparing the carbide slag leaching solution.

As a preferable scheme of the invention, the compound inducer is compounded by aluminum chloride, polyethylene glycol and sodium polyphosphate.

As a preferred embodiment of the present invention, the specific method for recycling the filtrate obtained in step 400 is:

and extracting and standing the obtained filtrate in a suction filtration mode, gradually adjusting the filtrate according to a preset gradient when the temperature of the filtrate is reduced to a preset temperature after standing, so as to meet the requirement of preparing the pH value of the nano calcium carbonate with different particle sizes, and adding the carbide slag again after adjusting the temperature and the pH value to enter the next cycle.

As a preferred aspect of the present invention, the step 200 further includes:

step 201, arranging a plurality of concentric annular areas in the normal pressure reaction kettle;

202, adding the carbide slag leaching solution into the normal-pressure reaction kettle, so that the carbide slag leaching solution is divided into a plurality of parts to be filled into the annular areas respectively;

step 203, raising all the annular areas, and enabling each annular area to be distributed on different heights;

and 204, filling the annular regions with the dioxide one by one for carbonization, so that precipitation reactions occur in different annular regions successively.

In order to solve the above technical problems, the present invention further provides the following technical solutions:

a preparation device comprises a reaction kettle body for containing the carbide slag leaching solution, a temperature control device for adjusting the temperature in the reaction kettle body to a preset temperature, a gas control device for introducing carbon dioxide into the reaction kettle body, a pressure control device for adjusting the air pressure in the reaction kettle body to be unchanged when the gas control device introduces carbon dioxide, a stirring device and a pH monitoring module for monitoring the pH value of the reaction solution in real time so as to stop the introduction of the carbon dioxide into the gas control device when the pH value reaches a preset value.

As a preferable scheme of the present invention, the pressure control device includes a buffer heating cavity formed in the reaction kettle, a pressure stabilizing heating cavity is nested in the buffer heating cavity, a pressure increasing valve is disposed on one side of the pressure stabilizing heating cavity, and a pressure reducing valve is disposed on the other side of the pressure stabilizing heating cavity.

As a preferred scheme of the invention, the stirring device comprises a rotary telescopic shaft body arranged in the pressure-stabilizing heating cavity, the top end of the rotary telescopic shaft body penetrates through the pressure-stabilizing heating cavity and is rotatably mounted on the reaction kettle body, and a stepped bearing cavity for unfolding when the rotary telescopic shaft body rotates and folding when the rotary telescopic shaft body is static is arranged at the bottom end of the rotary telescopic shaft body;

the stepped bearing cavity comprises a circular plate body fixedly mounted on the rotary telescopic shaft body, a first ring body is movably nested on the outer side of the circular plate body in a longitudinally slidable manner, and a second ring body is nested on the outer side of the first ring body in a longitudinally slidable manner;

the first ring body is circumferentially and uniformly provided with a plurality of first grooves, the second ring body is circumferentially and uniformly provided with a plurality of second grooves, the first grooves are in one-to-one correspondence with the second grooves, and the first grooves are connected with the corresponding second grooves through movable communicating structures.

As a preferable scheme of the present invention, the movable communicating structure includes a movable cavity opened on a side wall of the second groove close to the first groove, a communicating wall is installed in the movable cavity in a longitudinally telescopic manner through a first elastic resetting member, a pressure applying wall for pressing the communicating wall is installed on a side wall of the first groove close to the second groove, a flow channel is opened on the pressure applying wall, an end sealing plate is installed at one end of the flow channel close to the second groove in a longitudinally slidable manner through a second elastic resetting member, a through groove is opened at a position where the flow channel faces the end sealing plate, and a bottom end of the end sealing plate is hermetically nested in the through groove;

and an ejector plate which penetrates through the through groove and ejects the end sealing plate is arranged in the movable cavity, and a through hole is formed in the ejector plate.

As a preferable scheme of the present invention, the gas control device includes a primary and secondary movable door installed on the other side wall of the first groove or the second groove, a generating chamber for generating carbon dioxide and preheating the carbon dioxide is fixedly installed on the pressure stabilizing heating chamber, an arc-shaped groove is provided at the bottom end of the generating chamber, an electric telescopic hollow rod is slidably nested in the arc-shaped groove, an inner cavity of the electric telescopic hollow rod is communicated with the generating chamber through an elastic tube, one end of an elastic telescopic hollow rod is vertically connected to the bottom end of the electric telescopic hollow rod, the inner cavity of the elastic telescopic hollow rod is communicated with the inner cavity of the electric telescopic hollow rod, and a plug connector for butting with the primary and secondary movable door is fixedly installed at the other end of the elastic telescopic hollow rod.

As a preferable scheme of the present invention, air inlet channels are respectively disposed on the first groove and the second groove, the primary and secondary movable doors are disposed at outer ends of the air inlet channels, inner ends of the air inlet channels penetrate into inner cavities of the first groove or the second groove, and a pneumatic stirring assembly is mounted at inner ends of the air inlet channels; the pneumatic stirring assembly comprises a hollow shaft body which is sealed and rotatably arranged, a hollow stirring blade is arranged on the hollow shaft body in a communicated mode, and a water inlet preventing nozzle which is used for spraying carbon dioxide in a solution to drive the hollow stirring blade to rotate by utilizing the reaction of the sprayed carbon dioxide is arranged on the hollow stirring blade.

Compared with the prior art, the invention has the following beneficial effects:

the preparation process takes the carbide slag as a raw material, produces the nano calcium carbonate with higher added value, and has the advantages of environmental protection, good economic benefit and the like, the reaction process is sealed in the generation reaction process of the calcium carbonate so as to keep the air pressure and the temperature in the reaction process relatively stable, thus effectively controlling the solubility of the carbon dioxide, further maintaining the relatively stable pH value of the solution, leading the reaction to be more complete and leading the product to be close to the target form, and the invention carries out precipitation reaction on different areas in sequence by the zoned reaction in the normal pressure reaction kettle so as to reduce the influence of heat release or heat absorption generated in the reaction area on the unreacted area and assist in keeping the temperature relatively stable in the reaction process; the invention reduces the overflow of heat in the reaction kettle body by using the sealed normal-pressure reaction kettle body, but because the gas control device changes the air pressure in the normal-pressure reaction kettle body and then the pressure control device is used for preventing the change of the air pressure in the reaction kettle body, the invention can reduce the heat overflow and the true reaction temperature approaches the preset value when the reaction condition of the normal pressure is ensured.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.

FIG. 1 is a schematic process flow diagram of a preparation process in an embodiment of the present invention;

FIG. 2 is an XRD pattern of the nano-calcium carbonate product prepared in example 1;

FIG. 3 is an SEM image of the nano calcium carbonate product prepared in example 1;

FIG. 4 is an SEM image of the nano calcium carbonate product prepared in example 2;

FIG. 5 is an SEM image of the nano calcium carbonate product prepared in example 3;

FIG. 6 is an SEM image of the nano calcium carbonate product prepared in example 4;

FIG. 7 is a schematic view showing the overall configuration of a production apparatus according to an embodiment of the present invention;

FIG. 8 is an enlarged view of a portion of FIG. 7A according to an embodiment of the present invention;

FIG. 9 is a schematic view of a water inlet prevention nozzle according to an embodiment of the present invention.

The reference numerals in the drawings denote the following, respectively:

1-a reaction kettle body; 2-a gas control device; 3-a pressure control device; 4-temperature control device; 5-a stirring device;

21-primary and secondary movable doors; 22-generating a cavity; 23-an arc-shaped groove; 24-an electric telescopic hollow rod; 25-an elastic tube; 26-elastically telescoping hollow bar; 27-a plug-in unit;

31-buffer heating cavity; 32-a voltage-stabilizing heating cavity; 33-a pressure increasing valve; 34-a pressure relief valve;

51-a rotating telescopic shaft body; 52-stepped bearing and mounting cavity; 53-an intake passage; 54-a pneumatic stirring assembly;

521-a circular plate body; 522-a first ring body; 523-a second ring body; 524-first recess; 525-an active cavity; 526-a first resilient return member; 527-connecting wall; 528-pressing wall; 529-flow channel; 5210-a second resilient return member; 5211-end closure plate; 5212-a through slot; 5213-knock out plate; 5214-through the aperture; 5215-second groove;

541-a hollow shaft body; 542-hollow stirring blade; 543-water-inlet-proof nozzle.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

As shown in fig. 1 to fig. 6, the invention provides a preparation process for synthesizing nano calcium carbonate based on a composite inducer, which comprises the following steps:

The composite inducer is compounded by aluminum chloride, polyethylene glycol and sodium polyphosphate, and the mass ratio of the aluminum chloride to the polyethylene glycol to the sodium polyphosphate in the composite inducer is 1: 1-2.5: 2-5.

The specific method for recycling the filtrate obtained in step 400 is as follows:

Example 1: putting 100ml of leaching solution with calcium ion concentration of 0.8mol/L into a normal pressure reaction kettle, adding 0.1g of aluminum chloride, 0.12g of polyethylene glycol and 0.2g of sodium polyphosphate, uniformly mixing, stirring and introducing carbon dioxide at 14 ℃, stopping the reaction when the pH value of the solution reaches 8.5, filtering the reaction solution to obtain filtrate (ammonium chloride solution), and performing evaporation concentration crystallization to obtain an ammonium chloride sample; and washing and drying the obtained filter cake to obtain a nano calcium carbonate sample. The nano calcium carbonate prepared by detection is metastable calcite + vaterite type, and the particle size is 20-40 nm.

Example 2:

putting 100ml of leaching solution with calcium ion concentration of 1mol/L into a normal pressure reaction kettle, adding 0.15g of aluminum chloride, 0.2g of polyethylene glycol and 0.3g of sodium polyphosphate, uniformly mixing, stirring and introducing carbon dioxide at 22 ℃, stopping the reaction when the pH value of the solution reaches 7.5, filtering the reaction solution to obtain filtrate (ammonium chloride solution), and performing evaporation concentration crystallization to obtain an ammonium chloride sample; and washing and drying the obtained filter cake to obtain a nano calcium carbonate sample. The nano calcium carbonate prepared by detection is metastable calcite + vaterite type, and the particle size is 30-45 nm.

Example 3:

putting 100ml of leaching solution with calcium ion concentration of 1.1mol/L into a normal pressure reaction kettle, adding 0.1g of aluminum chloride, 0.15g of polyethylene glycol and 0.3g of sodium polyphosphate, uniformly mixing, stirring and introducing carbon dioxide at 10 ℃, stopping the reaction when the pH value of the solution reaches 8, filtering the reaction solution to obtain filtrate (ammonium chloride solution), and performing evaporation concentration crystallization to obtain an ammonium chloride sample; and washing and drying the obtained filter cake to obtain a nano calcium carbonate sample. The nano calcium carbonate prepared by detection is metastable calcite + vaterite type, and the particle size is 20-60 nm.

Example 4:

putting 100ml of leaching solution with calcium ion concentration of 1.2mol/L into a normal pressure reaction kettle, adding 0.1g of aluminum chloride, 0.25g of polyethylene glycol and 0.3g of sodium polyphosphate, uniformly mixing, stirring and introducing carbon dioxide at 25 ℃, stopping the reaction when the pH value of the solution reaches 8, filtering the reaction solution to obtain filtrate (ammonium chloride solution), and performing evaporation concentration crystallization to obtain an ammonium chloride sample; and washing and drying the obtained filter cake to obtain a nano calcium carbonate sample. The nano calcium carbonate prepared by detection is metastable calcite + vaterite type, and the particle size is 20-60 nm.

From the 4 examples above, it can be seen that changing the concentration of the leaching solution, the predetermined temperature of the reaction, and the predetermined pH will change the particle size of the product.

The calcium ion concentration in the primary circulating filtrate obtained in step 401 is reduced due to the participation of the calcium ion in the reaction, and when the circulating times of the circulating filtrate are gradually increased, the calcium ion concentration in the circulating filtrate is gradually reduced, so that the reaction preset temperature and the preset pH value are correspondingly changed, and the particle size of the product particles can be directionally changed.

In the process, the reaction process is sealed in the reaction process of generating the calcium carbonate so as to keep the air pressure and the temperature in the reaction process relatively stable, thereby effectively controlling the solubility of the carbon dioxide and further maintaining the pH value of the solution relatively stable, so that the reaction is more complete and the product can approach the target form.

As shown in fig. 7-9, the present invention further provides a preparation apparatus, which includes a reaction vessel 1 for containing the carbide slag leaching solution, a temperature control device 4 for adjusting the temperature in the reaction vessel 1 to a preset temperature, a gas control device 2 for introducing carbon dioxide into the reaction vessel 1, a pressure control device 3 for adjusting the pressure in the reaction vessel 1 to be constant when the gas control device 2 is introduced with carbon dioxide, a stirring device 5, and a pH monitoring module for monitoring the pH value of the reaction solution in real time to stop the introduction of carbon dioxide into the gas control device 2 when the pH value reaches a preset value.

The device is a process for realizing constant temperature and constant pressure in the scheme.

The sealed normal pressure reaction kettle body 1 is used to reduce the overflow of heat in the reaction kettle body 1, but the gas control device 2 changes the air pressure in the normal pressure reaction kettle body 1, and the pressure control device 3 is used to prevent the change of the air pressure in the reaction kettle body 1, so that the heat overflow and dispersion are reduced when the reaction condition of the normal pressure is ensured, and the real reaction temperature approaches the preset value.

Wherein, pressure control device 3 is including forming in the buffering heating chamber 31 in the reation kettle body 1 buffering heating chamber 31 is interior nested has steady voltage heating chamber 32 one side of steady voltage heating chamber 32 is provided with pressure-increasing valve 33 the opposite side of steady voltage heating chamber 32 is provided with relief valve 34.

The pressure increasing valve 33 is composed of an opening arranged on the upper inner side of the pressure stabilizing heating cavity 32 and a magnetic plate which can be adsorbed on the opening, the top end of the magnetic plate is rotatably connected on the pressure stabilizing heating cavity 32, and the pressure reducing valve 34 is similar to the pressure reducing valve.

Wherein, agitating unit 5 is including setting up in the rotatory flexible axis body 51 in steady voltage heating chamber 32, the top of rotatory flexible axis body 51 is run through steady voltage heating chamber 32 and is rotated and install on the reation kettle body 1, and the bottom of rotatory flexible axis body 51 is provided with and is used for the rotatory flexible axis body 51 to rotate the time and expand, fold when static cascaded dress chamber 52 that holds that folds. The stepped bearing cavity 52 comprises a circular plate 521 fixedly mounted on the rotary telescopic shaft 51, a first ring 522 movably nested on the outer side of the circular plate 521 in a longitudinally slidable manner, and a second ring 523 nested on the outer side of the first ring 522 in a longitudinally slidable manner. A plurality of first grooves 524 are circumferentially and uniformly formed in the first ring member 522, a plurality of second grooves 5215 are circumferentially and uniformly formed in the second ring member 523, the first grooves 524 correspond to the second grooves 5215 one to one, and the first grooves 524 are connected to the corresponding second grooves 5215 through a movable communicating structure.

The movable communicating structure comprises a movable cavity 525 which is arranged on one side wall of the second groove 5215 close to the first groove 524, a communicating wall 527 is longitudinally and telescopically arranged in the movable cavity 525 through a first elastic resetting piece 526, a pressure applying wall 528 which is used for pressing the communicating wall 527 is arranged on one side wall of the first groove 524 close to the second groove 5215, a flow channel 529 is arranged on the pressure applying wall 528, a blocking plate 5211 is longitudinally and slidably arranged at one end of the flow channel 529 close to the second groove 5215 through a second elastic resetting piece 5210, a through groove 5212 is arranged at a position where the flow channel 529 is opposite to the blocking plate 5211, and the bottom end of the blocking plate 5211 is hermetically nested in the through groove 5212. An ejector plate 5213 for penetrating the through groove 5212 and ejecting the end cap 5211 is installed in the movable chamber 525, and a through hole 5214 is opened in the ejector plate 5213.

The rotary telescopic shaft body 51 is longitudinally telescopic to control the expansion and contraction of the stepped bearing cavity 52, and when the rotary telescopic shaft body 51 ascends, the stepped bearing cavity 52 is expanded.

The expanding and closing of the stepped bearing cavity 52 means that when the stepped bearing cavity 52 is closed, the first groove 524 on the stepped bearing cavity 52 is communicated with the second groove 5215, and the leaching solution can be filled into the second groove 5215 only by filling the leaching solution into the first groove 524.

When the stepped bearing cavity 52 is expanded, the first groove 524 and the second groove 5215 are separated from each other, so that the first groove 524 and the second groove 5215 are not interfered with each other, and the reaction temperature of an unreacted region can be prevented from being interfered by an endothermic or exothermic process generated in a reaction region, thereby ensuring the stability of the reaction temperature.

Wherein the gas control device 2 comprises a primary and secondary movable door 21 installed on the other side wall of the first groove 524 or the second groove 5215, a generating chamber 22 for generating carbon dioxide and preheating the carbon dioxide is fixedly installed on the pressure stabilizing heating chamber 32, an arc-shaped groove 23 is arranged at the bottom end of the generating cavity 22, an electric telescopic hollow rod 24 is nested in the arc-shaped groove 23 in a sliding way, and the inner cavity of the electric telescopic hollow rod 24 is communicated with the generating cavity 22 through an elastic tube 25, one end of an elastic telescopic hollow rod 26 is vertically connected to the bottom end of the electric telescopic hollow rod 24, and the inner cavity of the elastic telescopic hollow rod 26 is communicated with the inner cavity of the electric telescopic hollow rod 24, and a plug connector 27 for butting with the primary and secondary movable doors 21 is fixedly arranged at the other end of the elastic telescopic hollow rod 26.

The plug connector 27 is nested on the primary and secondary movable doors 21 to inflate the leaching solution, and the stepped bearing cavity 52 rotates, so that the electric telescopic hollow rod 24 rotates along with the stepped bearing cavity 52

Due to the limitation of the arc-shaped groove 23, the electric telescopic hollow rod 24 cannot rotate continuously, so the plug connector 27 is nested in the other primary and secondary movable door 21 under the action of the elastic telescopic hollow rod 26, and drives the electric telescopic hollow rod 24 to move reversely, and similarly, the other primary and secondary movable doors 21 are inflated, and the process that the electric telescopic hollow rod 24 rotates along with one of the stepped bearing cavities 52 is the inflation time of carbon dioxide.

Through the design of the special shape of the gas control device 2, only the telescopic length of the electric telescopic hollow rod 24 needs to be controlled, so that the gas control device 2 can be controlled to inflate any sub-part of the stepped bearing cavity 52, and the sequence of the reaction of the inner sub-parts of the stepped bearing cavity 52 is controlled.

By changing the rotating speed of the electric telescopic hollow rod 24, the aeration time of the carbon dioxide can be controlled, and the aeration time of the carbon dioxide is controlled, so that the pH value of the solution can be reduced until the carbon dioxide in the solution is saturated, that is, the size of the preset pH value is controlled to a certain extent, and a foundation is provided for changing the reaction condition in the cyclic reaction process of the leaching solution.

The first groove 524 and the second groove 5215 are both provided with an air inlet channel 54, the primary and secondary movable doors 21 are disposed at the outer end of the air inlet channel 54, the inner end of the air inlet channel 54 penetrates into the inner cavity of the first groove 524 or the second groove 5215, and the inner end of the air inlet channel 54 is provided with a pneumatic stirring assembly 55. The pneumatic stirring assembly 55 includes a hollow shaft 551 which is hermetically and rotatably installed, a hollow stirring blade 552 which is communicatively installed on the hollow shaft 551, and a water inlet prevention nozzle 553 which is opened on the hollow stirring blade 552 and is used for ejecting carbon dioxide in a solution to drive the hollow stirring blade 552 to rotate by a reaction of the ejected carbon dioxide.

The water inlet prevention nozzle 553 is a structure that is automatically opened by the impact of high pressure and automatically closed by the action of low pressure, and provides power for stirring of the device through the aeration process of carbon dioxide, thereby reducing energy consumption.

The above embodiments are only exemplary embodiments of the present application, and are not intended to limit the present application, and the protection scope of the present application is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present application and such modifications and equivalents should also be considered to be within the scope of the present application.

Claims

1. A preparation process for synthesizing nano calcium carbonate based on a composite inducer is characterized by comprising the following steps: the method comprises the following steps:

step 100: dissolving ammonium chloride powder into deionized water, adding carbide slag, and removing solid impurities in a reaction solution after complete reaction at room temperature to obtain a carbide slag leaching solution;

step 300: after the precipitation process is finished, carrying out solid-liquid separation on the reaction solution to obtain a filter cake;

step 400: and washing and drying the filter cake to obtain a nano calcium carbonate sample, wherein the obtained filtrate is an ammonium chloride solution and is circularly used for preparing the carbide slag leaching solution.

2. The preparation process for synthesizing nano calcium carbonate based on the composite inducer, according to claim 1, is characterized in that: the compound inducer is compounded by aluminum chloride, polyethylene glycol and sodium polyphosphate.

3. The preparation process for synthesizing nano calcium carbonate based on the composite inducer, according to claim 2, is characterized in that: the specific method for recycling the filtrate obtained in step 400 is as follows:

and extracting and standing the obtained filtrate in a suction filtration mode, gradually adjusting the filtrate according to a preset gradient when the temperature of the filtrate is reduced to a preset temperature after standing, so as to meet the requirement of preparing the pH values of the nano calcium carbonate with different particle sizes, and adding the carbide slag again after adjusting the temperature and the pH value to enter the next cycle.

4. The preparation process of the nano calcium carbonate based on the composite inducer, according to claim 3, is characterized in that: the step 200 further comprises:

5. A production apparatus used in the production process according to any one of claims 1 to 4, characterized in that: including being used for holding the reation kettle body (1) of carbide slag leaching solution, be used for adjusting temperature to temperature control device (4) of predetermineeing the temperature in the reation kettle body (1), be used for to control gas device (2) that lets in carbon dioxide in the reation kettle body (1), be used for adjusting when controlling gas device (2) lets in carbon dioxide the unchangeable accuse pressure device (3), agitating unit (5) of reation kettle body (1) internal gas pressure, the pH value that is used for real-time supervision reaction solution stop when pH reaches the default accuse gas device (2) let in the pH monitoring module of carbon dioxide.

6. A manufacturing apparatus as set forth in claim 5, wherein: accuse pressure equipment (3) including form in buffering heating chamber (31) in the reation kettle body (1) the nested steady voltage heating chamber (32) that has in buffering heating chamber (31) one side in steady voltage heating chamber (32) is provided with pressure-increasing valve (33) the opposite side in steady voltage heating chamber (32) is provided with relief pressure valve (34).

7. A manufacturing apparatus as set forth in claim 6, wherein: the stirring device (5) comprises a rotary telescopic shaft body (51) arranged in the pressure-stabilizing heating cavity (32), the top end of the rotary telescopic shaft body (51) penetrates through the pressure-stabilizing heating cavity (32) and is rotatably installed on the reaction kettle body (1), and a stepped bearing cavity (52) used for unfolding when the rotary telescopic shaft body (51) rotates and folding when the rotary telescopic shaft body (51) is static is arranged at the bottom end of the rotary telescopic shaft body (51);

the stepped bearing cavity (52) comprises a circular plate body (521) fixedly mounted on the rotary telescopic shaft body (51), a first ring body (522) is movably nested on the outer side of the circular plate body (521) in a longitudinally slidable manner, and a second ring body (523) is nested on the outer side of the first ring body (522) in a longitudinally slidable manner;

a plurality of first grooves (524) are circumferentially and uniformly formed in the first ring body (522), a plurality of second grooves (5215) are circumferentially and uniformly formed in the second ring body (523), the first grooves (524) are in one-to-one correspondence with the second grooves (5215), and the first grooves (524) are connected with the corresponding second grooves (5215) through movable communication structures.

8. A manufacturing apparatus as set forth in claim 7, wherein: the movable communication structure comprises a movable cavity (525) which is arranged on the side wall of the second groove (5215) close to the first groove (524), a communication wall (527) is longitudinally and telescopically arranged in the movable cavity (525) through a first elastic resetting piece (526), a pressing wall (528) for pressing the communication wall (527) on a side wall of the first groove (524) near the second groove (5215), a flow channel (529) is arranged on the pressure applying wall (528), one end of the flow channel (529) close to the second groove (5215) is provided with a sealing plate (5211) in a longitudinally sliding way through a second elastic reset piece (5210), a through groove (5212) is arranged at the position of the flow channel (529) opposite to the sealing plate (5211), the bottom end of the end sealing plate (5211) is hermetically nested in the through groove (5212);

an ejector plate (5213) for penetrating the through groove (5212) and ejecting the end sealing plate (5211) is installed in the movable cavity (525), and a through hole (5214) is formed in the ejector plate (5213).

9. A manufacturing apparatus as set forth in claim 8, wherein: accuse gas device (2) is including installing primary and secondary dodge gate (21) on first recess (524) or the opposite side lateral wall of second recess (5215) go up fixed mounting and generate carbon dioxide and carry out the formation chamber (22) that preheats carbon dioxide generate the bottom in chamber (22) be provided with arc wall (23) slidable ground nests in arc wall (23) and has electronic flexible hollow rod (24), just the inner chamber of electronic flexible hollow rod (24) with generate chamber (22) and be linked together through elasticity pipe (25) the bottom of electronic flexible hollow rod (24) is connected with the one end of the hollow rod of elastic stretching out and drawing back (26) perpendicularly, just the inner chamber of the hollow rod of elastic stretching out and drawing back (26) with the inner chamber of the hollow rod of electronic flexible (24) communicates each other the other end fixed mounting of the hollow rod of elastic stretching out and drawing back (26) be used for with the inserting of butt joint of primary and secondary dodge gate (21) is inserted A connecting piece (27).

10. A manufacturing apparatus as set forth in claim 9, wherein: air inlet channels (53) are respectively formed in the first groove (524) and the second groove (5215), the primary and secondary movable doors (21) are arranged at the outer ends of the air inlet channels (53), the inner end of each air inlet channel (53) penetrates into the inner cavity of the first groove (524) or the second groove (5215), and a pneumatic stirring assembly (54) is installed at the inner end of each air inlet channel (53);

the pneumatic stirring assembly (54) comprises a hollow shaft body (541) which is sealed and rotatably arranged, a hollow stirring blade (542) is arranged on the hollow shaft body (541) in a communicating mode, and a water inlet prevention nozzle (543) used for spraying carbon dioxide in a solution to drive the hollow stirring blade (542) to rotate by utilizing the reaction of the sprayed carbon dioxide is arranged on the hollow stirring blade (542).