CN113171632A - Method for removing impurity gas in carbide slag slurry by micro-nano bubbles - Google Patents

Method for removing impurity gas in carbide slag slurry by micro-nano bubbles Download PDF

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CN113171632A
CN113171632A CN202110723960.0A CN202110723960A CN113171632A CN 113171632 A CN113171632 A CN 113171632A CN 202110723960 A CN202110723960 A CN 202110723960A CN 113171632 A CN113171632 A CN 113171632A
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carbide slag
slag slurry
micro
acetylene
water source
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CN113171632B (en
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朱干宇
李会泉
孟子衡
李少鹏
颜坤
杨悦
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Institute of Process Engineering of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/0073Degasification of liquids by a method not covered by groups B01D19/0005 - B01D19/0042
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/0036Flash degasification
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/0042Degasification of liquids modifying the liquid flow
    • B01D19/0052Degasification of liquids modifying the liquid flow in rotating vessels, vessels containing movable parts or in which centrifugal movement is caused
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/06Jet mills
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/18Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
    • B02C19/186Use of cold or heat for disintegrating
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10HPRODUCTION OF ACETYLENE BY WET METHODS
    • C10H21/00Details of acetylene generators; Accessory equipment for, or features of, the wet production of acetylene

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a method for removing impurity gas in carbide slag slurry by micro-nano bubbles, which comprises the following steps: (1) the gas source and the carbide slag slurry as the water source enter the micro-nano bubble generating device to generate the carbide slag slurry containing micro-nano bubbles; (2) degassing the carbide slag slurry containing the micro-nano bubbles to remove impurity gases in the carbide slag slurry; the impurity gas contains acetylene. The method of the invention utilizes the special effect of the micro-nano bubbles during generation and destruction, effectively removes acetylene and special odor gas in the carbide slag slurry, avoids the possible safety risk in the carbide slag utilization process, and has the advantages of high degassing speed, good effect, simple equipment, low cost and the like.

Description

Method for removing impurity gas in carbide slag slurry by micro-nano bubbles
Technical Field
The invention belongs to the technical field of resources and environment, and particularly relates to a method for removing impurity gas in carbide slag slurry by micro-nano bubbles.
Background
The carbide slag is industrial waste generated in the process of preparing acetylene by reacting carbide with water, the main component of the carbide slag is calcium hydroxide, and the carbide slag can be directly used in cement, building materials and the like, or used as a desulfurizing agent or used for preparing active calcium oxide and the like after separation and purification. In recent years, more and more researches have been carried out on carbide slag which has high calcium content and low price.
Acetylene in the dry and wet acetylene sludge exists in the forms of adsorbed acetylene, acetylene wrapped by acetylene sludge, dissolved acetylene and the like. The acetylene coated by the carbide slag is acetylene generated by further hydrolyzing unreacted carbide particles, and the unreacted carbide particles are coated inside the particles, so that the acetylene is released slowly. In the process of resource utilization of the dry and wet carbide slag, acetylene escapes and is enriched, and particularly in a closed/semi-closed space, if the acetylene is excessively accumulated, a great potential safety hazard is brought to the production process. Aiming at the explosion-proof problem of residual acetylene gas in carbide slag, the pretreatment operation of removing acetylene in the carbide slag is needed before the carbide slag is recycled.
CN105219435A discloses a method for recovering acetylene from slag slurry, in which, the overflow of a generator is sent to a slag slurry tank through a closed pipeline, and then sent to a desorption tower by a slag slurry pump, and the carbide slag slurry is subjected to low-pressure boiling desorption in the desorption tower; collecting the acetylene gas after desorption. The overflow pipe of the generator in the method is a closed pipeline, and the problem that the original overflow tank is unsafe in the open air is solved. However, the method adopts low-pressure boiling desorption to recover acetylene gas, has high requirements on the sealing property of equipment and has high recovery cost.
CN208327922U discloses a device of automatic desorption acetylene from carbide slag thick liquid, including the sediment thick liquid jar, the inside heating coil that sets up of sediment thick liquid jar, the sediment thick liquid jar passes through the sediment thick liquid pump and connects the desorption tower, the pipeline passes through the slurry return pipe between sediment thick liquid pump and the desorption tower and connects the sediment thick liquid jar, set up the governing valve on the slurry return pipe, the connection cooler of sediment thick liquid jar and desorption tower, the bottom export of desorption tower and cooler connects gas-tight groove and liquid-tight groove respectively, gas-tight groove and liquid-tight groove connect the row of cinder pond, the water ring vacuum pump is connected to the cooler, water ring vacuum pump connects oxygen on-line analyzer, oxygen on-line analyzer connects first blast pipe and second blast pipe respectively, set up the trip valve on first blast pipe and the second blast pipe, the acetylene buffer tank is connected to the second blast pipe, the acetylene output tube is connected to the acetylene buffer tank. However, the device has a low acetylene removal rate, and a certain potential safety hazard exists because more acetylene still remains in the treated carbide slag slurry.
CN209815990U discloses a dry-method carbide slag acetylene gas and silicon iron recycling device, which comprises a dry-method carbide slag pretreatment device, an acetylene gas generation device, a silicon iron recovery device and an acetylene gas purification device, wherein the dry-method carbide slag pretreatment device consists of a closed spiral, a small bag-type dust remover, a carbide slag tank, a nitrogen tank, a Roots blower, an airflow dry heat device and a lifter, the closed spiral and the small bag-type dust remover are arranged above the carbide slag tank, and the airflow dry heat device is arranged below the carbide slag tank; the device effectively solves the problems of resource waste, environmental pollution and potential safety hazard caused by the fact that the acetylene sludge produced by the dry method contains the calcium carbide and the silicon iron in the prior art. But the device has complex composition and large floor area.
In the methods, no special odor gas such as hydrogen sulfide or phosphine in dry carbide slag and/or wet carbide slag is considered to be removed, and acetylene still has a high residual quantity, so that no relevant research is carried out on the removal of residual acetylene in the carbide slag after acetylene is recovered. Therefore, it is required to develop a method for removing impurity gases from dry and wet carbide slag, which has simple equipment, low treatment cost and high removal efficiency.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a method for removing impurity gases in carbide slag slurry by using micro-nano bubbles, which utilizes the special effect of the micro-nano bubbles during generation and destruction to release acetylene dissolved in the carbide slag slurry and refine carbide slag particles, thereby realizing removal of carbide acetylene wrapped by carbide slag, avoiding the possible safety risk of dry and wet carbide slag during the utilization process, and simultaneously removing special odor gases in the carbide slag slurry.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for removing impurity gas in carbide slag slurry by micro-nano bubbles, which comprises the following steps:
(1) the gas source and the carbide slag slurry as the water source enter the micro-nano bubble generating device to generate the carbide slag slurry containing micro-nano bubbles;
(2) degassing the carbide slag slurry containing the micro-nano bubbles to remove impurity gases in the carbide slag slurry; the impurity gas contains acetylene.
The invention utilizes the high-speed rotation and injection of the gas source and water source mixed fluid in the production process of the micro-nano bubbles to generate strong shearing and high-frequency pressure change; when the micro-nano bubbles are broken out, the pressure is instantly released to form ultrahigh-speed micro jet flow and local ultrahigh temperature, so that acetylene dissolved in the carbide slag slurry is released, carbide slag particles can be further broken, the fine carbide slag particles are more favorable for fully contacting carbide slag wrapped carbide acetylene with water, the acetylene is quickly released, the concentration of residual acetylene gas in the carbide slag slurry is reduced, and the safety problem of dry and wet carbide slag in the subsequent utilization process is avoided.
The micro-nano bubbles refer to bubbles with the diameter less than or equal to 1mm, and the common bubbles refer to bubbles with the diameter more than 1 mm.
Preferably, the carbide slag slurry in the step (1) comprises carbide slag slurry and/or wet carbide slag slurry prepared by mixing dry carbide slag and water.
The dry carbide slag is produced in the process of preparing acetylene by using calcium carbide as a raw material by a dry method, and is required to be mixed with water to prepare carbide slag slurry.
The method can directly use the conventional wet carbide slag slurry produced in the process of preparing acetylene by using the wet method and using the calcium carbide as the raw material without other treatment.
Preferably, the mass content of the carbide slag in the carbide slag slurry is 1% to 30%, and may be, for example, 1%, 3%, 5%, 10%, 15%, 20%, 25%, or 30%.
Preferably, the particle size of the carbide slag in the carbide slag slurry is 1-800 μm, for example, 1-100 μm, 1-200 μm, 1-300 μm, 1-400 μm, 1-500 μm or 1-800 μm.
The method can be used for treating the carbide slag slurry containing carbide slag particles with the particle size range of 1-800 mu m, and the micro-nano bubbles can generate strong shearing and ultrahigh-speed micro jet flow in the generation and breaking processes to break the carbide slag particles.
Preferably, the volume of acetylene in the carbide slag slurry as a water source in the step (1) is 0.005-1 mL, and may be, for example, 0.005mL, 0.01mL, 0.05mL, 0.08mL, 0.1mL or 1 mL.
Preferably, the size of the micro-nano bubbles in the carbide slag slurry containing the micro-nano bubbles in the step (1) is 100nm to 100 μm, for example, 100nm, 300nm, 500nm, 1 μm, 10 μm or 100 μm.
The micro-nano bubbles are generated by a micro-nano bubble generating device, and the sizes of the micro-nano bubbles are all in the range of 100 nm-100 mu m. The acetylene sludge removal device is formed by an air source and the carbide slag slurry, and the carbide slag slurry containing micro-nano bubbles in the interval range can be used for efficiently removing acetylene, hydrogen sulfide and phosphine through subsequent degassing treatment.
Preferably, the ratio of the volume of the carbide slag slurry as the water source entering the micro-nano bubble generating device per hour in the step (1) to the volume of the carbide slag slurry in the degassing treatment is 1 (0.1-10.0), and may be, for example, 1:0.1, 1:0.5, 1:1.0, 1:2.0, 1:3.0, 1:5.0, 1:7.0, 1:9.0 or 1: 10.0.
Preferably, the volume flow rate of the gas source in the step (1) is 2.0% -10.0% of the volume flow rate of the carbide slag slurry as the water source, and may be, for example, 2.0%, 2.5%, 3.0%, 4.0%, 5.0%, 8.0%, 9.0% or 10.0%.
The volume flow of the air source is 2.0% -10.0% of the volume flow of the carbide slag slurry as the water source, because when the volume flow of the air source is less than 2.0% of the volume flow of the carbide slag slurry as the water source, the number of formed micro-nano bubbles is small; when the volume flow of the air source is more than 10.0 percent of the volume flow of the carbide slag slurry as the water source, the micro-nano bubbles can be polymerized to form large bubbles, which is not beneficial to removing acetylene, hydrogen sulfide and phosphine in the carbide slag slurry.
Preferably, the gas source comprises any one or a combination of at least two of air, oxygen, nitrogen or ozone, with typical but non-limiting combinations being air and oxygen, oxygen and nitrogen, nitrogen and ozone or air, oxygen and nitrogen, preferably ozone.
In the invention, the gas source is preferably oxidizing gas ozone, so that the removal effect of special odor gas dissolved in the carbide slag slurry can be further improved.
Preferably, the carbide slag slurry as the water source in the step (1) is degassed before entering the micro-nano bubble generation device.
Before the carbide slag slurry as the water source enters the micro-nano bubble generating device, the carbide slag slurry is degassed to remove part of the adsorbed acetylene and dissolved acetylene which are easy to remove in the carbide slag slurry, so that the removal rate of the acetylene in the carbide slag slurry is improved.
Preferably, the impurity gas in the step (2) further contains hydrogen sulfide and/or phosphine.
Preferably, the degassing treatment of step (2) is performed under ventilation conditions.
The degassing treatment is preferably carried out under the ventilation condition, the removal rate of acetylene, hydrogen sulfide and phosphine can be accelerated through gas flow, and the removal effect of impurity gases in the carbide slag slurry is improved.
Preferably, the ventilation air volume is 1000-5000 m3H, for example, may be 1000m3/h、1500m3/h、2000m3/h、2500m3/h、3000m3/h、4000m3H or 5000m3/h。
Preferably, the ventilation air pressure is 60-400 Pa, such as 60Pa, 80Pa, 100Pa, 150Pa, 280Pa, 310Pa or 400 Pa.
Preferably, the degassing treatment of step (2) is performed under stirring conditions.
Preferably, the stirring speed is 50-200 rpm, for example, 50rpm, 70rpm, 100rpm, 130rpm, 150rpm, 170rpm or 200 rpm.
Preferably, the degassing treatment time in the step (2) is 1 min-6 h, and for example, may be 1min, 10min, 30min, 1h, 3h, 4h, 5h or 6 h.
Preferably, the temperature of the degassing treatment is 20 to 90 ℃, for example, 20 ℃, 40 ℃, 50 ℃, 60 ℃, 80 ℃ or 90 ℃.
In the invention, the temperature of the degassing treatment is preferably controlled to be 20-90 ℃, and the degassing treatment can be realized by arranging a heating device at the bottom of the degassing device or directly introducing hot carbide slag slurry.
Preferably, the carbide slag slurry after the degassing treatment in the step (2) is subjected to solid-liquid separation to obtain purified carbide slag and a separation liquid.
In the invention, the carbide slag slurry after the degassing treatment can be continuously discharged from the degassing device or intermittently discharged.
The carbide slag slurry after degassing treatment needs to be subjected to solid-liquid separation, so that the moisture in the carbide slag slurry is removed, the volume of the carbide slag slurry is reduced, and the subsequent transportation and use are facilitated.
The solid-liquid separation according to the present invention is not particularly limited, and any method known to those skilled in the art that can be used for solid-liquid separation, for example, filtration, sedimentation, centrifugation, or the like, can be used.
The separation liquid can be returned to be used as water for preparing the carbide slag slurry by mixing with the dry carbide slag for recycling, so that the treatment cost can be reduced.
In the invention, the carbide slag slurry after the degassing treatment in the step (2) is preferably returned to the step (1) to be used as a water source for recycling, and solid-liquid separation is carried out after at least two circulations, so that the acetylene in the carbide slag slurry can be removed to the maximum extent.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) the method comprises the following steps that an air source and carbide slag slurry serving as a water source enter a micro-nano bubble generating device to generate the carbide slag slurry containing micro-nano bubbles, wherein the size of the micro-nano bubbles is 100 nm-100 mu m; the volume of acetylene in each milliliter of the carbide slag slurry as a water source is 0.005-1 mL; the volume flow of the gas source is 2.0% -10.0% of the volume flow of the carbide slag slurry as a water source; the method comprises the following steps that the carbide slag slurry as a water source is subjected to degassing treatment before entering a micro-nano bubble generating device;
(2) ventilating the carbide slag slurry containing the micro-nano bubbles at the temperature of 20-90 ℃, and degassing for 1 min-6 h to remove impurity gases in the carbide slag slurry; the impurity gas contains acetylene; the impurity gas also contains hydrogen sulfide and/or phosphine; the ratio of the volume of the carbide slag slurry as a water source entering the micro-nano bubble generating device per hour to the volume of the carbide slag slurry in degassing treatment is 1 (0.1-10.0).
The recitation of numerical ranges herein includes not only the above-recited values, but also any values between any of the above-recited numerical ranges not recited, and for brevity and clarity, is not intended to be exhaustive of the specific values encompassed within the range.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method for removing the impurity gas in the carbide slag slurry by the micro-nano bubbles provided by the invention realizes the high-efficiency removal of acetylene in the carbide slag slurry, has high removal speed and good removal effect, and has the acetylene removal rate of more than or equal to 56.76 percent and the acetylene removal rate of more than or equal to 99.90 percent under better conditions;
(2) the method for removing the impurity gas in the carbide slag slurry by the micro-nano bubbles synchronously removes special odor gas in the carbide slag slurry, the removal rate of hydrogen sulfide is more than or equal to 48.90%, and the removal rate of hydrogen sulfide is more than or equal to 99.80% under better conditions; the removal rate of phosphine is more than or equal to 46.98 percent, the removal rate of phosphine is more than or equal to 99.87 percent under the optimal condition, and the purified carbide slag obtained under the optimal condition has no peculiar smell.
Drawings
Fig. 1 is a schematic diagram of a method and a device for removing impurity gases in carbide slag slurry by using micro-nano bubbles.
In the figure: 1-micro-nano bubble generating device; 2-a degassing device; 3-a solid-liquid separation device; 4-air volume conveying device; 5-a stirring device; 6-carbide slag slurry feeding pipe; 7-water source feeding pipe; 8, an air source air inlet pipe; 9-a carbide slag slurry discharge pipe containing micro-nano bubbles; 10-an air inlet pipe; 11-an air outlet pipe; 12-discharging pipe after degassing treatment; 13-purifying the carbide slag discharging pipe; 14-a separation liquid outlet pipe.
Detailed Description
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The device adopted by the method for removing impurity gas from carbide slag slurry by micro-nano bubbles provided by the following embodiment is shown in fig. 1.
The device comprises a micro-nano bubble generating device 1, a degassing device 2, a solid-liquid separation device 3, an air volume conveying device 4 and a stirring device 5.
The stirring device 5 is arranged in the degassing device 2, and the air volume conveying device 4 is connected with the degassing device 2 through an air outlet pipeline 11.
The solid-liquid separation device 3 is connected with the degassing device 2 through a degassing treatment discharge pipe 12; the solid-liquid separation device 3 also comprises a purified carbide slag discharging pipe 13 and a separation liquid discharging pipe 14.
The device also comprises a water source feeding pipe 7, an air source air inlet pipe 8 and a carbide slag slurry discharging pipe 9 containing micro-nano bubbles, wherein the water source feeding pipe 7 is connected with the micro-nano bubble generator 1.
The apparatus also includes a carbide slurry feed pipe 6 and an air inlet pipe 10 connected to the degassing apparatus 2.
Example 1
The embodiment provides a method for removing impurity gas in carbide slag slurry by micro-nano bubbles, which comprises the following steps:
(1) wet carbide slag slurry with 10% of carbide slag mass content and 1-200 μm of particle size is firstly introduced into a degassing device, and then is used as a water source and enters a micro-nano bubble generating device with air, so as to generate the carbide slag slurry containing micro-nano bubbles with the size of 100 nm-100 μm; the volume of acetylene in each milliliter of the carbide slag slurry used as a water source is 0.008 mL; the volume flow of the air is 8.0% of the volume flow of the carbide slag slurry as a water source;
(2) the ventilation air volume of the carbide slag slurry containing the micro-nano bubbles is 3000m3Degassing for 3 hours under the conditions that the air pressure is 280Pa, the stirring speed is 100rpm and the temperature is 50 ℃, and removing impurity gases in the carbide slag slurry; the impurity gas contains acetylene; the impurity gas also contains hydrogen sulfide and/or phosphine; filtering the carbide slag slurry after the degassing treatment to obtain purified carbide slag and a separation liquid; the ratio of the volume of the carbide slag slurry as a water source entering the micro-nano bubble generating device per hour to the volume of the carbide slag slurry in degassing treatment is 1: 5.0.
Example 2
The embodiment provides a method for removing impurity gas in carbide slag slurry by micro-nano bubbles, which comprises the following steps:
(1) introducing carbide slag slurry with the mass content of 5% and the particle size range of 1-400 mu m into a degassing device, and then taking the carbide slag slurry as a water source and oxygen to enter a micro-nano bubble generating device to generate the carbide slag slurry containing micro-nano bubbles with the size of 100 nm-100 mu m; the carbide slag slurry is prepared by mixing dry carbide slag and water; the volume of acetylene in each milliliter of the carbide slag slurry used as a water source is 1 mL; the volume flow of the oxygen is 5.0% of the volume flow of the carbide slag slurry as a water source;
(2) the ventilation air volume of the carbide slag slurry containing the micro-nano bubbles is 4000m3Performing degassing treatment for 1h under the conditions of 310Pa of wind pressure, 150rpm of stirring speed and 40 ℃ of temperature to remove impurity gas in the carbide slag slurry; the impurity gas contains acetylene; the impurity gas also contains hydrogen sulfide and/or phosphine; and centrifuging the carbide slag slurry after the degassing treatment to obtain purified carbide slag and a separation liquid. Wherein the ratio of the volume of the carbide slag slurry as a water source entering the micro-nano bubble generating device per hour to the volume of the carbide slag slurry in degassing treatment is 1: 1.0;and (3) returning the separation liquid to the step (1) for recycling as water for preparing the carbide slag slurry.
Example 3
The embodiment provides a method for removing impurity gas in carbide slag slurry by micro-nano bubbles, which comprises the following steps:
(1) wet carbide slag slurry with the mass content of carbide slag being 20% and the particle size range being 1-100 mu m is firstly introduced into a degassing device, and then is used as a water source and enters a micro-nano bubble generating device with nitrogen, so as to generate the carbide slag slurry containing micro-nano bubbles with the size of 100 nm-100 mu m; the volume of acetylene in each milliliter of the carbide slag slurry used as a water source is 0.01 mL; the volume flow of the nitrogen is 2.0 percent of the volume flow of the carbide slag slurry as a water source;
(2) the ventilation air volume of the carbide slag slurry containing the micro-nano bubbles is 2000m3Degassing for 5 hours under the conditions that the air pressure is 100Pa, the stirring speed is 200rpm and the temperature is 60 ℃, and removing impurity gases in the carbide slag slurry; the impurity gas contains acetylene; the impurity gas also contains hydrogen sulfide and/or phosphine; filtering the carbide slag slurry after the degassing treatment to obtain purified carbide slag and a separation liquid; the ratio of the volume of the carbide slag slurry as a water source entering the micro-nano bubble generating device per hour to the volume of the carbide slag slurry in degassing treatment is 1: 0.5.
Example 4
The embodiment provides a method for removing impurity gas in carbide slag slurry by micro-nano bubbles, which comprises the following steps:
(1) introducing carbide slag slurry with the mass content of 1% and the particle size range of 1-800 mu m into a degassing device, and then taking the carbide slag slurry as a water source and oxygen to enter a micro-nano bubble generating device to generate the carbide slag slurry containing micro-nano bubbles with the size of 100 nm-100 mu m; the carbide slag slurry is prepared by mixing dry carbide slag and water; the volume of acetylene in each milliliter of the carbide slag slurry used as a water source is 0.05 mL; the volume flow of the oxygen is 3.0% of the volume flow of the carbide slag slurry as a water source;
(2) the micro-nano bubble-containingThe ventilation air volume of the carbide slag slurry is 5000m3Performing degassing treatment for 1min under the conditions of 400Pa of wind pressure, 200rpm of stirring speed and 90 ℃ of temperature to remove impurity gas in the carbide slag slurry; the impurity gas contains acetylene; the impurity gas also contains hydrogen sulfide and/or phosphine; and filtering the carbide slag slurry after the degassing treatment to obtain purified carbide slag and a separation liquid. Wherein the ratio of the volume of the carbide slag slurry as a water source entering the micro-nano bubble generating device per hour to the volume of the carbide slag slurry in degassing treatment is 1: 0.1; and (3) returning the separation liquid to the step (1) for recycling as water for preparing the carbide slag slurry.
Example 5
The embodiment provides a method for removing impurity gas in carbide slag slurry by micro-nano bubbles, which comprises the following steps:
(1) the method comprises the following steps of introducing wet carbide slag slurry with the carbide slag mass content of 30% and the particle size range of 1-300 mu m into a degassing device, taking the wet carbide slag slurry as a water source and ozone to enter a micro-nano bubble generating device, and generating the carbide slag slurry with micro-nano bubbles with the micro-nano bubble size of 100 nm-100 mu m; the volume of acetylene in each milliliter of the carbide slag slurry used as a water source is 0.005 mL; the volume flow of the ozone is 10.0% of the volume flow of the carbide slag slurry as a water source;
(2) the ventilation air volume of the carbide slag slurry containing the micro-nano bubbles is 1000m3Performing degassing treatment for 6 hours under the conditions that the air pressure is 60Pa, the stirring speed is 50rpm and the temperature is 20 ℃, and removing impurity gases in the carbide slag slurry; the impurity gas contains acetylene; the impurity gas also contains hydrogen sulfide and/or phosphine; and filtering the carbide slag slurry after the degassing treatment to obtain purified carbide slag and a separation liquid. Wherein the ratio of the volume of the carbide slag slurry as a water source entering the micro-nano bubble generating device per hour to the volume of the carbide slag slurry in degassing treatment is 1: 10.0.
Example 6
This embodiment provides a method for removing impurity gases from a carbide slag slurry by using micro-nano bubbles, which is the same as embodiment 1 except that the volume flow of air is 1.0% of the volume flow of the carbide slag slurry as a water source.
Example 7
This embodiment provides a method for removing impurity gases from a carbide slag slurry by using micro-nano bubbles, which is the same as embodiment 1 except that the volume flow of air is 15.0% of the volume flow of the carbide slag slurry as a water source.
Example 8
The embodiment provides a method for removing impurity gases in carbide slag slurry by micro-nano bubbles, which is the same as the embodiment 5 except that ozone is replaced by nitrogen.
Example 9
The embodiment provides a method for removing impurity gases in carbide slag slurry by micro-nano bubbles, which is the same as the embodiment 1 except that degassing treatment is not performed and ventilation is not performed.
Comparative example 1
The comparative example provides a method for removing impurity gases in carbide slag slurry by bubbles, and the method is the same as that in example 1 except that a micro-nano bubble generating device is replaced by a bubbling device to generate the carbide slag slurry containing bubbles with the bubble size of 1-10 mm.
The method for testing the acetylene release amount of the carbide slag comprises the following steps: mixing carbide slag slurry or purified carbide slag with water to prepare slurry with the same concentration as the original carbide slag slurry, adding the slurry into a sealed round-bottom flask, stirring for 6 hours at 40 ℃, detecting the concentration of acetylene released from the round-bottom flask, calculating the amount (mL) of acetylene released from the carbide slag, and calculating the amount (mL/mL) of acetylene released from the carbide slag according to the volume (mL) of the carbide slag slurry. Acetylene removal rate (%) = (acetylene release amount of the carbide slag before treatment-acetylene release amount of the carbide slag after treatment)/acetylene release amount of the carbide slag before treatment × 100.
The test method of hydrogen sulfide and phosphine comprises the following steps: the concentrations of hydrogen sulfide and phosphine in the released gas before and after the treatment of the carbide slag slurry are detected by using a gas chromatography.
The method for calculating the removal rate of hydrogen sulfide and phosphine comprises the following steps: hydrogen sulfide or phosphine removal rate (%) = (amount of released hydrogen sulfide or phosphine before treatment-amount of released hydrogen sulfide or phosphine after treatment)/amount of released hydrogen sulfide or phosphine before treatment × 100.
The raw carbide slag slurry and the purified carbide slag in examples 1 to 9 and comparative example 1 were subjected to sampling tests, and the test results are shown in table 1.
TABLE 1
Figure DEST_PATH_IMAGE001
From table 1, the following points can be seen:
(1) it can be seen from the comprehensive examples 1 to 9 that the method for removing impurity gases in the carbide slag slurry by using the micro-nano bubbles provided by the invention realizes the efficient removal of acetylene, hydrogen sulfide and phosphine in the carbide slag slurry, the acetylene removal rate is not less than 56.76%, and the acetylene removal rate is not less than 99.90% under better conditions; the removal rate of the hydrogen sulfide is more than or equal to 48.90 percent, and the removal rate of the hydrogen sulfide is more than or equal to 99.80 percent under better conditions; the removal rate of phosphine is more than or equal to 46.98 percent, the removal rate of phosphine is more than or equal to 99.87 percent under the optimal condition, and the purified carbide slag obtained under the optimal condition has no peculiar smell;
(2) it can be seen from the combination of examples 1 and 6 to 7 that, the volume flow rate of air in example 1 is 8.0% of the volume flow rate of the carbide slag slurry as the water source, and compared with the volume flow rates of air in examples 6 to 7 which are 1.0% and 15.0% of the volume flow rate of the carbide slag slurry as the water source, the acetylene removal rate in example 1 is 99.90%, the hydrogen sulfide removal rate is 97.40%, and the phosphine removal rate is 97.10%, the obtained purified carbide slag is odorless, while the air in example 6 is small, the amount of formed micro-nano bubbles is small, the acetylene removal rate is only 56.76%, the hydrogen sulfide removal rate is only 48.90%, and the phosphine removal rate is only 46.98%, the obtained purified carbide slag has a nasal-prick odor, and a large amount of micro-nano bubbles are polymerized in example 7, so that the removal rates of acetylene, hydrogen sulfide and phosphine are greatly reduced, the acetylene removal rate is 85.66%, the hydrogen sulfide removal rate is 73.55%, the phosphine removal rate is 75.18%, and the obtained purified carbide slag has a slight odor; therefore, the proportional relation between the volume flow of the air source and the volume flow of the carbide slag slurry as a water source is further controlled, and a proper amount of micro-nano bubbles are generated, so that the acetylene, hydrogen sulfide and phosphine in the carbide slag slurry can be removed, and the micro-nano bubbles cannot form large bubbles;
(3) it can be seen from the combination of embodiment 5 and embodiment 8 that, in embodiment 5, ozone is introduced into the micro-nano bubble generation device as a gas source, and compared with the introduction of nitrogen in embodiment 8, in embodiment 5, the acetylene removal rate is 99.80%, the hydrogen sulfide removal rate is 99.80%, and the phosphine removal rate is 99.87%, the obtained purified carbide slag has no odor, while in embodiment 8, the acetylene removal rate is 97.60%, the hydrogen sulfide removal rate is significantly reduced to 66.45%, the phosphine removal rate is also reduced to 68.30%, and the obtained purified carbide slag has slight odor; therefore, the oxidizing gas ozone is further preferably selected as the gas source, so that the removal effect of the special odor gas in the carbide slag slurry can be improved;
(4) by combining example 1 and example 9, it can be seen that, when the degassing treatment is performed under the ventilation condition in example 1, compared with the degassing treatment in which no ventilation is performed in example 9, the acetylene removal rate, the hydrogen sulfide removal rate and the phosphine removal rate in example 1 are all higher than those in example 9, the purified carbide slag obtained in example 1 has no peculiar smell, and the purified carbide slag obtained in example 9 has slight peculiar smell; therefore, the invention further preferably carries out degassing treatment under the ventilation condition, accelerates the removal rate of acetylene, hydrogen sulfide and phosphine through gas flow, and improves the removal effect of impurity gas in the carbide slag slurry;
(5) it can be seen from the combination of the embodiment 1 and the comparative example 1 that the carbide slag slurry containing micro-nano bubbles with the micro-nano bubble size of 100nm to 100 μm is generated by adopting the micro-nano bubble generating device in the embodiment 1, compared with the carbide slag slurry containing bubbles with the bubble size of 1 to 10mm, which is generated by adopting the bubbling device in the comparative example 1, the acetylene removal rate in the comparative example 1 is only 25.71%, the hydrogen sulfide removal rate is only 31.50%, the hydrogen phosphide removal rate is only 30.90%, and the obtained purified carbide slag has pungent odor; therefore, the method provided by the invention has the advantages that the carbide slag slurry containing micro-nano bubbles is generated by the micro-nano bubble generating device and then is subjected to impurity gas removal, so that the acetylene, hydrogen sulfide and phosphine are efficiently removed.
In conclusion, the method for removing the impurity gas in the carbide slag slurry by the micro-nano bubbles provided by the invention realizes the efficient removal of the acetylene and the special odor gas hydrogen sulfide and phosphine in the carbide slag slurry, and avoids the possible safety risk in the utilization process of the dry and wet carbide slag.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. A method for removing impurity gases in carbide slag slurry by micro-nano bubbles is characterized by comprising the following steps:
(1) the gas source and the carbide slag slurry as the water source enter the micro-nano bubble generating device to generate the carbide slag slurry containing micro-nano bubbles;
(2) degassing the carbide slag slurry containing the micro-nano bubbles to remove impurity gases in the carbide slag slurry; the impurity gas contains acetylene.
2. The method according to claim 1, wherein the volume of acetylene in the carbide slag slurry as a water source in step (1) is 0.005-1 mL per mL.
3. The method according to claim 1 or 2, wherein the micro-nano bubbles in the carbide slag slurry containing micro-nano bubbles in the step (1) have a size of 100 nm-100 μm.
4. The method according to claim 3, wherein the ratio of the volume of the carbide slag slurry as the water source entering the micro-nano bubble generating device per hour in the step (1) to the volume of the carbide slag slurry in the degassing treatment is 1 (0.1-10.0).
5. The method of claim 1, wherein the volume flow rate of the gas source in step (1) is 2.0% to 10.0% of the volume flow rate of the carbide slag slurry as the water source.
6. The method according to claim 5, wherein the carbide slag slurry as the water source in the step (1) is degassed before entering the micro-nano bubble generation device.
7. The method according to claim 1, wherein the impurity gas of step (2) further contains hydrogen sulfide and/or phosphine.
8. The method of claim 1, wherein the degassing of step (2) is performed under aeration conditions.
9. The method according to claim 8, wherein the degassing treatment in the step (2) is carried out for 1 min-6 h;
the temperature of the degassing treatment is 20-90 ℃.
10. Method according to claim 1, characterized in that it comprises the following steps:
(1) the method comprises the following steps that an air source and carbide slag slurry serving as a water source enter a micro-nano bubble generating device to generate the carbide slag slurry containing micro-nano bubbles, wherein the size of the micro-nano bubbles is 100 nm-100 mu m; the volume of acetylene in each milliliter of the carbide slag slurry as a water source is 0.005-1 mL; the volume flow of the gas source is 2.0% -10.0% of the volume flow of the carbide slag slurry as a water source; the method comprises the following steps that the carbide slag slurry as a water source is subjected to degassing treatment before entering a micro-nano bubble generating device;
(2) stirring the carbide slag slurry containing the micro-nano bubbles under the conditions of ventilation and 20-90 ℃, and carrying out degassing treatment for 1 min-6 h to remove impurity gases in the carbide slag slurry; the impurity gas contains acetylene; the impurity gas also contains hydrogen sulfide and/or phosphine; the ratio of the volume of the carbide slag slurry as a water source entering the micro-nano bubble generating device per hour to the volume of the carbide slag slurry in degassing treatment is 1 (0.1-10.0).
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