CN111153426A - Method for producing superfine barium sulfate by using impinging stream - Google Patents

Method for producing superfine barium sulfate by using impinging stream Download PDF

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Publication number
CN111153426A
CN111153426A CN202010128216.1A CN202010128216A CN111153426A CN 111153426 A CN111153426 A CN 111153426A CN 202010128216 A CN202010128216 A CN 202010128216A CN 111153426 A CN111153426 A CN 111153426A
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pressure
reaction
impinging stream
product
solution
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李沁峰
朱宏禹
斯敏贵
李霞
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Daguan Huaxin Mining Co Ltd
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Daguan Huaxin Mining Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/46Sulfates
    • C01F11/462Sulfates of Sr or Ba
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

Abstract

The invention discloses a method for producing superfine barium sulfate by utilizing impinging stream, which can reduce the damage to a nozzle while reducing the particle size of a product, and comprises the following steps: a) will be provided with
Figure 696888DEST_PATH_IMAGE002
And
Figure 496217DEST_PATH_IMAGE004
preparing a saturated solution, wherein the temperature is 25-30 ℃, the pressure is 0.1Mpa, and the obtained saturated solution is filtered to remove impurities to obtain reaction liquid which is respectively stored in two pressure containers; b) the two pressure containers are communicated with a high-pressure pump, and when the high-pressure pump works, high-pressure gas is introduced into the two pressure containers; c) the bottom of the pressure vessel is respectively communicated with the impinging stream reactor, so that different reaction liquids collide in the impinging stream reactor to form a reaction product C1 with smaller granularity; d) putting the obtained reaction product C1 into an aging device for aging to obtain a productD1; e) and centrifuging the product D1 at a high speed, taking out the precipitate, washing the precipitate for 3 times by using water and acetone respectively, and drying the precipitate to obtain the final product.

Description

Method for producing superfine barium sulfate by using impinging stream
Technical Field
The invention belongs to the technical field of superfine powder preparation, and particularly relates to a method for producing superfine barium sulfate by utilizing an impinging stream.
Background
Barium sulfate (commonly called barite) is an important inorganic chemical product, has the characteristics of high specific gravity, opacity to rays, inertness, pure white, no toxicity and the like, can be used as a filling agent and an additive in coating and plastics, and also can be used as a medical representation, the barium sulfate is high-temperature resistant, acid resistant and alkali resistant, can improve the properties of materials such as impact resistance, corrosion resistance, high temperature resistance, space stability and the like as the additive, the particle size of superfine barium sulfate powder is controlled to be about 0.1 micron, which is about one two percent of that of common fine barium sulfate, and has special properties which are not possessed by the conventional coarse crystal materials due to small size, large specific surface and quantum size effect, and the outstanding characteristics are as follows: the product has excellent optical performance, good dispersibility, good adsorptivity, stable performance and strong aging resistance, thereby obviously improving the thermal stability, the wear resistance, the sound insulation and the radiation resistance of the product and improving the strength, the toughness and the glossiness of the product.
The physical method is mainly mechanical crushing, the chemical method is mainly liquid phase precipitation method, the physical crushing method can obtain micron-sized particles, but the particle size distribution of the product is uneven, the purity is not high, and the agglomeration of powder in the preparation process of the liquid phase method is serious, so that the particle size and the distribution of the particles are difficult to control; or providing a uniform supersaturation environment to allow the reaction system to nucleate uniformly, such as membrane dispersion precipitation, uniform precipitation and hypergravity.
The basic concept of the impinging stream is that two or more homogeneous or heterogeneous phase fluids flow and impinge against each other, and due to the inertia, one side of the fluid penetrates into the opposing fluid through the impinging surface to generate a highly turbulent region, thereby achieving a very good micromixing effectThe preparation of the superfine powder needs to provide a very high and uniform supersaturation environment, and the conditions can be created because the impinging stream has the characteristic of promoting micromixing; the process flow for producing the superfine barium sulfate by adopting the impinging stream comprises the following steps: are first separately configured
Figure 414150DEST_PATH_IMAGE002
And
Figure 128029DEST_PATH_IMAGE004
the solution is purified and then respectively injected into two storage tanks, then the two reactions enter an impinging stream reactor for rapid mixing reaction at a certain flow rate through an advection pump, and the reaction product is aged, centrifugally separated at a high speed, washed and dried to obtain a finished product, but the method is actually adopted and used for a period of time, and the nozzle at the discharge port is easy to block and difficult to clean, and needs to be frequently replaced, so that the production efficiency is affected, and meanwhile, the replacement cost is increased, after the blocked nozzle is analyzed, the particles mainly separated from the reaction liquid block the nozzle, and the particles are larger than the nozzle of the nozzle to block the nozzle, so the reaction liquid can separate out solid-phase particles, and the preparation of the reaction liquid is carried out at normal temperature and pressure, so the reaction liquid is easily affected by the external temperature, the lower the temperature, the more solid phase precipitates in the reaction solution, and clogging occurs.
Disclosure of Invention
The invention aims to provide a method for producing superfine barium sulfate by utilizing impinging stream, which not only can avoid frequent replacement of a nozzle due to blockage, but also can further reduce the particle size of a finished product.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for producing superfine barium sulfate by using impinging stream comprises the following steps:
a. will be provided with
Figure DEST_PATH_IMAGE005
Preparing into saturated solution at 25-30 deg.C and pressureFiltering the saturated solution under 0.1Mpa to remove impurities to obtain reaction solution A, storing in pressure vessel A, and mixing
Figure DEST_PATH_IMAGE007
Preparing saturated solution at the same temperature and pressure, filtering and removing impurities from the obtained saturated solution to obtain reaction liquid B, storing the reaction liquid B in a pressure container B, and adding ammonium polyacrylate solution which is equivalent to 10 percent (mass fraction) of the theoretical yield of barium sulfate into the reaction liquid A as a dispersing agent;
b. the two pressure containers are communicated with a high-pressure pump, and when the high-pressure pump works, high-pressure gas is introduced into the two pressure containers;
c. the bottoms of the pressure vessels are respectively communicated with the impinging stream reactor, so that different reaction liquids in the two pressure vessels collide in the impinging stream reactor to form a reaction product C1 with smaller granularity;
d. putting the obtained reaction product C1 into an aging device for aging to obtain a product D1;
e. and centrifuging the product D1 at a high speed of 4000r/min for 10min, taking out the precipitate, washing with water and acetone for 3 times respectively, and drying at 80 ℃ for 30min to obtain a final product e1, namely packaging and warehousing.
Further, the high-pressure pump pressurizes the pressure container, so that the pressure in the pressure container reaches 20-30 Mpa.
Further, the aging device is a constant temperature box, and the product C1 is heated and aged at the aging temperature of 90 ℃ for 1 hour.
Further, a heating device is arranged in the pressure container to heat the solution.
Furthermore, a heating wire is wound on a pipeline connected between the impinging stream reactor and the pressure vessel.
The invention has at least the following beneficial effects:
(1) the temperature of the reaction liquid before entering the impinging stream reactor is increased, and the higher the temperature is, the higher the solubility is, so that the reaction liquid can not be separated out due to the reduction of the solubility, and a nozzle can not be blocked.
(2) The two pressure vessels can be pressurized simultaneously by only using one high-pressure pump, so that the cost is saved, meanwhile, the reaction liquid is pressed into the impinging stream reactor by using the pressure of the high-pressure pump, the flow rate is higher, more liquid drops can be generated by impingement, a large number of tiny reaction environments are formed, and smaller particles are obtained.
(3) The impinging stream and the pressure gas dissolving technology are combined, so that the flow rate of the reaction liquid can be improved, more air can be additionally dissolved, the air is additionally dissolved in the reaction liquid, a large number of micro-bubbles can be separated out due to pressure reduction after the air enters the impinging stream reactor, the micro-bubbles are broken during impingement, the micro-mixing effect is improved, and when the micro-bubble generating device is used with an ultrasonic wave matched impinging stream reactor, the bubble generating effect through cavitation is the same, but the cost is lower and the noise is lower.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
In the drawings:
FIG. 1 schematically illustrates a production flow diagram of the present invention;
FIG. 2 is a TEM photograph of samples obtained in examples of the present invention, comparative examples 1 and 2.
Detailed Description
The technical solutions of the present invention are clearly and completely described below, and it is obvious that the described embodiments are some, not all, embodiments of the present invention; 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.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; the two components can be directly connected or indirectly connected through an intermediate medium, and the two components can be communicated with each other; the specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Examples
a. Will be provided with
Figure 815755DEST_PATH_IMAGE005
Preparing saturated solution at normal temperature and normal pressure, wherein the temperature is 25-30 deg.C, and the pressure is one atmosphere (0.1 Mpa), filtering the saturated solution to remove impurities to obtain reaction solution A, storing in a pressure container A, and mixing
Figure 273281DEST_PATH_IMAGE007
Preparing saturated solution at the same temperature and pressure, filtering and removing impurities from the obtained saturated solution to obtain reaction liquid B, storing the reaction liquid B in a pressure container B, wherein the pressure container is a sealed container, the pressure container can display the pressure value inside the pressure container after being connected with a pressure gauge in the prior art, the two pressure containers are respectively stored with prepared saturated reaction liquid, and ammonium polyacrylate solution which is equivalent to 10 percent of the theoretical yield (mass fraction) of barium sulfate is added into the reaction liquid A as a dispersing agent.
It is worth noting that: the pressure vessel is a pressure tank, and the pressure tank used in this embodiment is a customized pressure tank, which can withstand a pressure of up to 35Mpa, and has a structure substantially the same as that of the pressure tank in the prior art, except that: the discharge port is arranged at the bottom of the pressure tank, and the side wall of the pressure tank is provided with a connector communicated with the high-pressure pump.
b. Two pressure vessel all communicate with the high-pressure pump, and the high-pressure pump during operation lets in high-pressure gas simultaneously in to two pressure vessel, makes the inside pressure increase of pressure vessel, and pressure in two pressure vessel reaches 20~30Mpa, and at this moment, because pressure in the pressure vessel is far above atmospheric pressure, so the solubility of air in the solution has just also increased, has more air to dissolve in the solution.
It should be noted that: still be provided with heating device in two pressure vessel, come the solution through heating device and heat, the heating device who adopts in this embodiment is the heating wire of taking the temperature control function, heat 40 ℃ 2 ℃ with the solution, through the temperature that increases the solution, improve the solubility of solution in the reaction solution, unsaturated solution originally has become unsaturated solution under pressure vessel's high temperature high pressure, consequently can not separate out solid particle in pressure vessel, the problem of damage shower nozzle when also having avoided solid particle from the high-speed blowout in the shower nozzle.
c. The bottom of the pressure vessel is communicated with the impinging stream reactor, so that different reaction liquids in the two pressure vessels collide in the impinging stream reactor, two groups of reaction liquids are sprayed into the impinging stream reactor through a nozzle according to the impinging stream reaction principle, a turbulent flow area is formed after the two flows collide with each other, high shearing force and extrusion force can be generated by interaction and collision between the two flows, and therefore the flows are more refined, the intensity of the turbulent flow area of the flows is enhanced by the impinging stream technology, the generated shearing force can better disperse the flows, the contact area is increased, the two flows can fully react, and a reaction product C1 with smaller granularity is formed.
It should be noted that: the pipeline connected between the impinging stream reactor and the pressure vessel is provided with a heating wire with a temperature control function besides a switch, the heating wire is used for heating the connecting pipeline, so that the temperature of the solution is kept at 40 +/-2 ℃, and the condition that the solution is separated out of crystals in the process of flowing into the impinging stream reactor when the outside air is cold, and then the nozzle is damaged or blocked is avoided.
d. And putting the obtained reaction product C1 into an ageing device for ageing to obtain a product D1.
e. And centrifuging the product D1 at a high speed of 4000r/min for 10min, taking out the precipitate, washing with water and acetone for 3 times respectively, and drying at 80 ℃ for 30min to obtain a final product e1, namely packaging and warehousing.
As a preferred example, the aging apparatus is a thermostat and the product C1 is aged by heating at a temperature of 90 ℃ for a period of 1 hour.
Comparative example 1
a. Will be provided with
Figure 212287DEST_PATH_IMAGE002
Preparing a saturated solution at normal temperature and normal pressure, wherein the temperature is 25-30 ℃, the pressure is one atmosphere, filtering the obtained saturated solution to remove impurities to obtain a reaction solution A, storing the reaction solution A in a storage tank a, and similarly, preparing the reaction solution A into a saturated solution
Figure 88278DEST_PATH_IMAGE007
Preparing saturated solution at the same temperature and pressure, filtering and removing impurities from the obtained saturated solution to obtain reaction liquid B, storing the reaction liquid B in a storage tank B, wherein the storage tank is used for storing the reaction liquid, and a constant-flow pump is arranged on a pipeline, the bottom of which is connected with the impinging stream reactor, and can accelerate the discharge of the reaction liquid.
It is worth noting that: an ammonium polyacrylate solution as a dispersant in an amount corresponding to 10% (mass fraction) of the theoretical yield of barium sulfate was added to the reaction mixture A.
b. And opening the advection pumps and the pipeline switches of the two storage tanks simultaneously, and reacting the two reaction liquids in the impinging stream reaction liquid at an impinging speed of 0.25-0.33 m/s to obtain a product C2.
c. The bottom of the pressure vessel is communicated with the impinging stream reactor, so that different reaction liquids in the two pressure vessels collide in the impinging stream reactor, two groups of reaction liquids are sprayed into the impinging stream reactor through a nozzle according to the impinging stream reaction principle, a turbulent flow area is formed after the two flows collide with each other, high shearing force and extrusion force can be generated by interaction and collision between the two flows, and therefore the flows are more refined, the intensity of the turbulent flow area of the flows is enhanced by the impinging stream technology, the generated shearing force can better disperse the flows, the contact area is increased, the two flows can fully react, and a reaction product C2 with smaller granularity is formed.
d. And putting the obtained reaction product C2 into an aging device for aging at the aging temperature of 90 ℃ for 1 hour to obtain a product D2.
e. And centrifuging the product D2 at a high speed of 4000r/min for 10min, taking out the precipitate, washing with water and acetone for 3 times respectively, and drying at 80 ℃ for 30min to obtain a final product e2, namely packaging and warehousing.
Comparative example 2
a. Will be provided with
Figure 417628DEST_PATH_IMAGE002
Preparing a saturated solution at normal temperature and normal pressure, wherein the temperature is 25-30 ℃, the pressure is one atmosphere, filtering the obtained saturated solution to remove impurities to obtain a reaction solution A, storing the reaction solution A in a pressure container A, and preparing the reaction solution A into a saturated solution at normal temperature and normal pressure
Figure 678845DEST_PATH_IMAGE007
Preparing saturated solution at the same temperature and pressure, filtering and removing impurities from the obtained saturated solution to obtain reaction liquid B, storing the reaction liquid B in a pressure container B, wherein the pressure container is the same as the embodiment, can display the pressure value inside the pressure container after being connected with a pressure gauge in the prior art, and the two pressure containers are respectively stored with the prepared saturated reaction liquid.
It is worth noting that: an ammonium polyacrylate solution as a dispersant in an amount corresponding to 10% (mass fraction) of the theoretical yield of barium sulfate was added to the reaction mixture A.
b. Two pressure vessel all communicate with the high-pressure pump, and the high-pressure pump during operation lets in high-pressure gas in to two pressure vessel, makes the inside pressure increase of pressure vessel, and pressure in two pressure vessel reaches 20~30Mpa, and at this moment, because the pressure in the pressure vessel is far above atmospheric pressure, so the solubility of air in the solution has just also increased, has more air to dissolve in the solution.
c. The bottom of the pressure vessel is communicated with the impinging stream reactor, so that different reaction liquids in the two pressure vessels collide in the impinging stream reactor, two groups of reaction liquids are sprayed into the impinging stream reactor through a nozzle according to the impinging stream reaction principle, a turbulent flow area is formed after the two flows collide with each other, high shearing force and extrusion force can be generated by interaction and collision between the two flows, and therefore the flows are more refined, the intensity of the turbulent flow area of the flows is enhanced by the impinging stream technology, the generated shearing force can better disperse the flows, the contact area is increased, the two flows can fully react, and a reaction product C3 with smaller granularity is formed.
d. And putting the obtained reaction product C3 into an ageing device for ageing to obtain a product D3.
e. And centrifuging the product D3 at a high speed of 4000r/min for 10min, taking out the precipitate, washing with water and acetone for 3 times respectively, and drying at 80 ℃ for 30min to obtain a final product e3, namely packaging and warehousing.
Examples of the experiments
Experimental materials: sodium sulfate, analytically pure, to become a research institute of urban combined chemical reagents; barium chloride, analytically pure, beijing beibeijing beijing fine chemicals llc; polyacrylic acid, chemically pure, shanghai-research biotechnology limited; ammonia, analytically pure, Chengdu Bosheng chemical Co., Ltd; acetone, analytically pure, hong sheng detection instrument limited company in Dongguan; absolute ethanol, analytically pure, atoz fine chemicals ltd.
Experimental equipment: a pressure pump with an output pressure of 30Mpa and a model of GSX100A, Shanghai Xiamen compressor, Inc.; a low-speed freezing centrifuge with model number of TDL-5000cR, Shanghai' an pavilion scientific instrument factory; a drying box with the model of 101-0BS, Hunan Lichen Instrument science and technology Limited; liquid-liquid impinging stream reactor model NP-PRLL21, Nawei science and technology (Shenzhen) Limited; transmission electron microscopy, model Philips CM 120.
The experimental method comprises the following steps: the experiment is carried out according to the embodiment, the comparison example 1 and the comparison example 2 respectively, samples are obtained respectively, the experiment is repeated for four times, only three groups of samples are randomly selected from the obtained five groups of samples due to the limitation of objective conditions, the appearance of the sample particles is observed through a transmission electron microscope, and the particle size is measured through image processing software according to a scale.
The values obtained are tabulated and explained below:
TABLE 1 particle size (. mu.m) of samples obtained by different preparation methods
Figure DEST_PATH_IMAGE009
Firstly, the difference between the comparative example 1 and the comparative example 2 is that the comparative example 2 presses the reaction liquid in the pressure vessel into the impinging stream reactor by the high-pressure pump, while the comparative example 1 adopts the advection pump to press the reaction liquid, the comparative example 1 is a method generally adopted in the prior art, but two reaction liquids need to adopt two pumps, so that the cost is increased, on the other hand, the pressure of the advection pump is limited, only the impinging speed of 0.25-0.33 m/s can be ensured, and the comparative example 2 and the embodiment adopt a method of pressing the reaction liquid by the high-pressure pump, compared with the traditional method, the method only needs to use one pump, the pressure which can be generated by the high-pressure pump is very large, the experimental process can visually judge that the speed of the reaction liquid which is pressed out by the high-pressure pump is higher than the liquid outlet speed of the advection pump, it is obvious from the data in table 1 that, after the impact velocity is increased, the particle size of the obtained sample is smaller because the higher the ejection velocity of the reaction solution is, the larger the kinetic energy carried by the reaction solution is, and when two streams of fluid impact, the shape of the impact region generated between the two streams of fluid will change with the difference of the impact strength, which indicates that the turbulence degree varies with the difference of the impact strength of the reaction solution, and when the impact strength is small, the turbulence degree is small, the two streams of fluid will flow out in a superposed manner after impacting, the region where the streams converge forms a "Y" shape, and the higher the flow velocity of the reaction solution, when the flow velocity in comparative example 1 is reached, an ultra-thin liquid surface will be formed on the converging surface of the two streams of fluid, and if the flow degree of the reaction solution is further increased, a cluster of ultra-thin mist droplets will be formed near the impact position, and the ultra-thin liquid surface will be formed or the generated mist droplets, the formation of fine and uniform particles is facilitated, so that the particle size of the barium sulfate obtained by the method of pressing out the reaction solution with high-pressure gas is smaller.
In addition, before the reaction liquid is extruded by high-pressure gas, the reaction liquid and the high-pressure gas are stored in a pressure container, the pressure value of the pressure container is as high as 30mpa, the solubility of air in the reaction liquid is increased, namely more air is dissolved in the solution of the reaction liquid, the solubility is increased, when the reaction liquid is sprayed out of the pressure container, due to the fact that the air pressure is reduced, the air dissolved in the solution is separated out in the form of micro-nano bubbles due to the increase of the pressure after the reaction liquid leaves a nozzle and is uniformly distributed in the reaction liquid, when two liquid flows collide with each other, the micro-nano bubbles are partially broken, and the rest liquid flows further reduce the size of mist liquid drops, so that a product with smaller particle size can be obtained, and under the double effects of pressure gas dissolving and high-speed collision, the particle size of the finally obtained product is obviously smaller than that of the traditional method, the use effect is better.
Three TEM photographs shown in fig. 2 are photographs taken from each of the samples prepared by the methods of example, comparative example 1, and comparative example 2, specifically: the sample obtained by the method of example 1 is marked at the top left corner in FIG. 2 as a, the sample obtained by the method of comparative example 2 is marked at the top left corner in FIG. 2 as b, the barium sulfate particles in graph a have smaller particle size and are dispersed more uniformly, the large particles therein are smaller and have no substantial agglomeration, the particles in graph b have relatively larger particle size and simultaneously have a substantial agglomeration, the agglomeration forms larger particle groups, which is equivalent to increasing the particle size, and the particles in graph c have better dispersion, which is between graph a and graph c and is generally similar to graph a, and the reaction solution ejection conditions of comparative example 2 and example are the same in combination with the above analysis, the difference is that the heating device is added in the embodiment, the heating device does not influence the spraying speed of the reaction liquid, and the pressurized and sprayed reaction liquid has higher spraying speed and larger kinetic energy, so that a finer reaction environment is formed in an impact area, particles with smaller particle size can be generated, and agglomeration is not easy to occur due to the smaller reaction environment, so that the reaction liquid has better dispersibility.
Further, in the case of performing the test, the same nozzle was used for a plurality of experimental groups using the same production method, and the nozzles used for different test methods were different from each other, and the use of the nozzle was observed 1 time, 3 times, and 5 times, and the results were as follows:
TABLE 2 service conditions of the spray heads after repeated tests
Figure DEST_PATH_IMAGE011
The difference between the above-mentioned embodiment and the comparative example 2 is that a heating device is added, that is, the heating device is installed on the pressure vessel and the pipeline between the pressure vessel and the impinging stream reactor, the heating device can increase the temperature of the reaction solution, thereby increasing the solubility of the solution in the reaction solution, and avoiding the precipitation of the solute therein at low temperature, table 2 is the data obtained by performing experiments with the most easily occurring scratch and blockage during the use as reference indexes after a plurality of sets of experiments, it is obvious from the table that, under the limited experiment times, only the nozzle in the comparative example 1 is slightly blocked, but the other two comparative examples are not present, after the analysis, the solution is prepared at normal temperature because the experiment time is positive in winter, the external temperature is too low, and the experiment environment is not subjected to heat preservation measures, crystals can be precipitated due to supersaturation at low temperature, particularly at the position of a pipeline where a storage tank is connected with the impinging stream reactor in the comparative example 1, the temperature reduction speed is higher and the crystals are more easily precipitated due to the fact that the surface area of the pipeline is larger and the heat exchange between the reaction liquid and the outside is more frequent in the flowing process, and the larger crystals can block a nozzle in the spraying process.
While comparative example 2 also shows no clogging, but comparative example 2 differs from comparative example 1 only in that the reaction liquid is pressed out by a high-pressure pump, and therefore the reason why no clogging occurs is that the solubility of the reaction liquid is increased by the high-pressure pump, on the other hand, the flow rate of the reaction liquid pressed out by the high-pressure pump is higher, and the high-pressure liquid flow ejects the liquid clogged at the nozzle under the pressure even if clogging occurs, so clogging is not likely to occur, but the pressure is not a main factor influencing the solubility of the solution, and the temperature is a main influence factor, so the influence of the pressure on the solubility is limited, and in the case that the external temperature is sufficiently low, the solution under the high-pressure environment is likely to precipitate crystals, and the method of forcibly ejecting the crystals from the nozzle by the high pressure easily forms scratches on the surface of the nozzle, and corrosion progresses from the scratch position to other positions as the degree of use increases, the use of the whole nozzle is further influenced, the embodiment mainly ensures the constant temperature of the reaction liquid through an external heating device, fundamentally avoids the influence of the external environment on the solubility of the reaction liquid, and therefore, crystals cannot be precipitated to damage the nozzle, and the service life of the nozzle can be effectively prolonged.

Claims (5)

1. A method for producing superfine barium sulfate by using impinging stream is characterized by comprising the following steps: the method comprises the following steps:
a. will be provided with
Figure 844199DEST_PATH_IMAGE002
Preparing a saturated solution, wherein the temperature is 25-30 ℃, the pressure is 0.1Mpa, filtering the obtained saturated solution to remove impurities to obtain a reaction solution A, storing the reaction solution A in a pressure container A, and mixing the reaction solution A with the reaction solution A
Figure 899880DEST_PATH_IMAGE004
Preparing saturated solution at the same temperature and pressure, filtering and removing impurities from the obtained saturated solution to obtain reaction liquid B, storing the reaction liquid B in a pressure container B, and adding ammonium polyacrylate solution which is equivalent to 10 percent (mass fraction) of the theoretical yield of barium sulfate into the reaction liquid A as a dispersing agent;
b. the two pressure containers are communicated with a high-pressure pump, and when the high-pressure pump works, high-pressure gas is introduced into the two pressure containers;
c. the bottoms of the pressure vessels are respectively communicated with the impinging stream reactor, so that different reaction liquids in the two pressure vessels collide in the impinging stream reactor to form a reaction product C1 with smaller granularity;
d. putting the obtained reaction product C1 into an aging device for aging to obtain a product D1;
e. and centrifuging the product D1 at a high speed of 4000r/min for 10min, taking out the precipitate, washing with water and acetone for 3 times respectively, and drying at 80 ℃ for 30min to obtain a final product e1, namely packaging and warehousing.
2. The method for producing ultra-fine barium sulfate using impinging stream as claimed in claim 1, wherein: and pressurizing the pressure container by the high-pressure pump to enable the pressure in the pressure container to reach 20-30 Mpa.
3. The method for producing ultra-fine barium sulfate using impinging stream as claimed in claim 1, wherein: the aging device is a constant temperature box, and the product C1 is heated and aged at the aging temperature of 90 ℃ for 1 hour.
4. The method for producing ultra-fine barium sulfate using impinging stream as claimed in claim 1, wherein: and the pressure container is also internally provided with a heating device for heating the solution.
5. The method for producing ultra-fine barium sulfate according to claim 4, wherein: and a heating wire is also wound on a pipeline connected between the impinging stream reactor and the pressure vessel.
CN202010128216.1A 2020-02-28 2020-02-28 Method for producing superfine barium sulfate by using impinging stream Pending CN111153426A (en)

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CN112852189A (en) * 2021-01-21 2021-05-28 山东联科科技股份有限公司 Preparation method of carbon black
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