CN112080753A - Carbon anode plate for fluorine preparation by impregnation method and tail gas treatment process - Google Patents
Carbon anode plate for fluorine preparation by impregnation method and tail gas treatment process Download PDFInfo
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- CN112080753A CN112080753A CN202010965908.1A CN202010965908A CN112080753A CN 112080753 A CN112080753 A CN 112080753A CN 202010965908 A CN202010965908 A CN 202010965908A CN 112080753 A CN112080753 A CN 112080753A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/245—Fluorine; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B15/00—Preventing escape of dirt or fumes from the area where they are produced; Collecting or removing dirt or fumes from that area
- B08B15/02—Preventing escape of dirt or fumes from the area where they are produced; Collecting or removing dirt or fumes from that area using chambers or hoods covering the area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
Abstract
The invention discloses a carbon anode plate for fluorine preparation by using an impregnation method and a tail gas treatment process, which comprises the following steps: drying the cut carbon anode plate green blank, then arranging the green blank in an impregnation tank in order, preheating, vacuumizing the impregnation tank, sucking impregnation liquid prepared by mixing solid phenolic resin and liquid acetone into the impregnation tank for impregnation, curing and roasting, and forming a protective layer on the surface of the carbon anode plate green blank so as to prevent the carbon anode plate from forming a C-F polymer layer on the surface of the carbon anode plate in the long-time use process of an electrolytic tank, wherein the carbon anode plate treated by the method is not easy to break, and the service life of the carbon anode plate is prolonged; the invention carries out cooling and dust-settling treatment on water used by a circular saw in the cutting process of the green material of the carbon anode plate, and utilizes a condensation recovery system to recover and treat the waste gas containing acetone in the pressure relief process of the impregnation tank.
Description
Technical Field
The invention relates to the technical field of semiconductor materials, in particular to a carbon anode plate for processing fluorine by using an impregnation method and a tail gas treatment process.
Background
The simple substance fluorine is an indispensable main raw material in the field of semiconductor manufacturing, a medium-temperature electrolysis method is generally adopted for producing fluorine gas, and an anode plate material adopted in a medium-temperature electrolysis tank is an important electrode product in fluoride electrolysis. Because the simple substance fluorine is extremely active, the fluorine preparation technology and the safety device have high difficulty and high requirement. The characteristics of the electrode for electrolytic production of fluorine are as follows: the electrolyte has the advantages of good resistance to corrosion of fluorine and hydrogen fluoride, low resistivity, good wettability of the electrolyte, small overvoltage, high mechanical strength, capability of being used under high current density for a long time, large specific gravity, capability of being locally crushed into fragments and sinking to the bottom of an electrolytic bath, capability of avoiding short circuit between electrodes, convenience in manufacturing, low price and the like. The carbon anode material for medium-temp. electrolytic fluorine-making electrolytic tank is made up by mixing ground calcined petroleum coke and coal pitch according to a certain proportion, forming and roasting (or soaking and roasting for two or more times). The manufacturing method has the disadvantages that because the strength of the carbon anode is not enough, when the electrolytic cell runs for a long time, a C-F polymer layer is formed on the surface of the carbon anode, so that the resistance is increased, the phenomena of anode polarization, carbon anode fracture and the like are easy to generate, a large amount of impurity gas is generated, the service time of the carbon anode is shortened, the production period is prolonged, and the production cost is increased; and tail gas is generated in the processing process of the carbon anode plate, so that the production environment is polluted.
Disclosure of Invention
The invention aims to provide a carbon anode plate for fluorine preparation by using an impregnation method and a tail gas treatment process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a carbon anode plate for fluorine preparation by using an impregnation method and a tail gas treatment process comprise the following steps:
step one, processing a carbon anode plate raw blank: cutting an outsourced carbon anode plate green body according to a specified size by using a circular saw, putting the cut green body into an oven, and drying the green body for 24 hours at the temperature of 120 ℃; cooling and dedusting a saw blade of the circular saw by using water in the cutting process, and collecting the generated wastewater to a wastewater tank for precipitation and recycling;
step two, dipping the carbon anode plate raw blank: in a paint storage tank, the mass ratio of 1: 1, adding solid phenolic resin and liquid acetone in proportion to prepare impregnation liquid, neatly arranging the dried carbon anode plate green blank in an impregnation tank, preheating to 80 ℃, vacuumizing the impregnation tank to 200-500 pa, sucking the impregnation liquid in a paint storage tank into the impregnation tank, controlling the temperature of the impregnation liquid to 80 ℃, stopping sucking the impregnation liquid when the liquid level of the impregnation liquid is 50mm higher than the top of the carbon anode plate green blank, pressurizing the impregnation tank to 0.5Mpa, and maintaining the pressure for 5 hours; taking out the raw blank of the carbon anode plate, scraping off redundant impregnation liquid on the surface of the raw blank of the carbon anode plate, and drying in the shade for 24 hours; pouring the impregnation liquid into the paint storage tank again for reuse;
step three, curing the carbon anode plate raw blank: putting the carbon anode plate raw blank processed in the step two into the impregnation tank again, boosting the pressure in the impregnation tank to 5Mpa, heating to 140-160 ℃ according to a set raw blank curing temperature-rising curve, curing for 20-30h, releasing the pressure and cooling the impregnation tank after curing is finished, and taking out the carbon anode plate raw blank; in the pressure relief process of the impregnation tank, a condensation recovery system is used for recovering and treating the discharged acetone-containing waste gas, and the acetone collected by the condensation recovery system is poured into the impregnation tank for recycling;
step four, roasting the carbon anode plate green blank: placing the solidified carbon anode plate raw blanks into a well-type resistance furnace at intervals of 20-30cm for roasting, filling the adjacent carbon anode plate raw blanks with quartz sand, and roasting at the temperature of 320-380 ℃ according to a set raw blank roasting temperature rise curve; and after roasting, naturally cooling the carbon anode plate to room temperature, and then using the carbon anode plate.
Preferably, the oven heating mode in the first step is steam heating.
Preferably, the raw material curing temperature rise curve in the third step is as follows: the temperature is increased from room temperature to 50 ℃ at a constant speed within the first 10 hours, then is increased from 50 ℃ to 80 ℃ at a constant speed within 3 hours, then is increased from 80 ℃ to 120 ℃ at a constant speed within 10 hours, and finally is increased from 120 ℃ to 150 ℃ at a constant speed within 6 hours.
Preferably, a discharge port of the condensation recovery system in the third step is connected with an activated carbon adsorption system, and the condensed gas is adsorbed by activated carbon again and then discharged to the outside through an exhaust funnel; the waste active carbon is recycled after recovery treatment.
Preferably, the green billet roasting temperature rise curve in the fourth step is as follows: uniformly raising the temperature from room temperature to 120 ℃ within the first 10 hours, uniformly raising the temperature from 120 ℃ to 350 ℃ within the last 10 hours, and finally keeping the temperature constant for 5 hours.
Preferably, the carbon anode plate treated in the fourth step needs to be drilled and tapped by a lathe, a gas collecting hood and an exhaust fan are arranged above the lathe, a small amount of dust generated in the drilling and tapping processes is sucked into a water bath pool and is precipitated by a water bath, and the requirement of environmental protection is met.
In the third step of the invention, the green blank is solidified and heated, the carbon plate is impregnated by the impregnation liquid prepared from solid phenolic resin and acetone, and the carbon plate has the advantages of improved thermal property, increased mechanical strength, high carbon residue rate, good rheological property, good physical compatibility between the carbon plate and electrolyte and the like mainly through the impregnation effect. In the first heating stage, the temperature is uniformly and slowly increased to 50 ℃ within 10 hours, and the impregnation liquid can be uniformly and slowly immersed into the carbon plate; in the second heating stage, the temperature is uniformly increased to 80 ℃ within 3 hours, the impregnation liquid is rapidly gasified (the boiling point temperature of acetone is 56.5 ℃), and the impregnation effect in the later stage is facilitated; and the third temperature rise stage and the fourth temperature rise stage rise the temperature at constant speed for 10 hours and 6 hours, so that the impregnation liquid can enter the carbon plate more deeply, and free aldehyde and free phenol carried by high-boiling-point acetone in the impregnation liquid can better enter the carbon plate.
In the fourth step of the invention, the green blank is roasted and heated, and the resin in the impregnated carbon plate is completely cured, so that the obtained carbon plate product has the characteristics of enhanced compactness, increased mechanical strength and the like. Heating to 120 ℃ at a constant speed in the first heating stage for 10 hours, and quickly gasifying acetone in the carbon plate (the boiling point temperature of the acetone is 56.5 ℃) to separate out; in the second heating stage, the temperature is uniformly raised to 350 ℃ within 10 hours, and acetone in the carbon plate is more thoroughly separated out; the third roasting stage is constant temperature for 5 hours, the phenolic resin is further stably solidified, the compactness of the carbon plate product is enhanced, and the mechanical strength is increased.
The invention has the beneficial effects that:
(1) the method comprises the steps of drying a cut carbon anode plate green blank, impregnating, curing and roasting by using acetone and phenolic resin, and forming a protective layer on the surface of the carbon anode plate green blank so as to prevent the carbon anode plate from forming a C-F polymer layer on the surface of the carbon anode plate in the long-time use process of an electrolytic tank;
(2) the method comprises the steps of cooling water for a circular saw and reducing dust in the cutting process of a green material of the carbon anode plate, recovering and treating the discharged acetone-containing waste gas by using a condensation recovery system in the pressure relief process of the impregnation tank, and adsorbing harmful gas by using active carbon, wherein the dust generated by sucking a gas collecting hood and an exhaust fan in the processing process of the carbon anode plate is used for protecting the environment in the processing process and meeting the requirement of environmental protection;
(3) according to the invention, redundant impregnation liquid on the surface of the carbon anode plate is scraped after green materials are impregnated, and acetone collected by a condensation recovery system is poured into an impregnation tank for recycling; the waste activated carbon is recycled, so that the waste of materials is effectively reduced, and resources are saved.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a graph of green carbon anode plate material curing temperature rise;
FIG. 3 is a graph of the firing temperature rise of the cured green carbon anode plate material.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
As shown in fig. 1, a carbon anode plate for fluorine production by using an immersion method and a tail gas treatment process include the following steps:
a carbon anode plate for preparing fluorine by using an impregnation method and a tail gas treatment process comprise the following steps:
step one, processing a carbon anode plate raw blank: cutting an outsourced carbon anode plate green body according to a specified size by using a circular saw, putting the cut green body into an oven, and drying the green body for 24 hours at the temperature of 120 ℃; cooling and dedusting a saw blade of the circular saw by using water in the cutting process, and collecting the generated wastewater to a wastewater tank for precipitation and recycling;
step two, dipping the carbon anode plate raw blank: in a paint storage tank, the mass ratio of 1: 1, adding solid phenolic resin and liquid acetone in proportion to prepare impregnation liquid, neatly arranging the dried carbon anode plate green blank in an impregnation tank, preheating to 80 ℃, vacuumizing the impregnation tank to 200-500 pa, sucking the impregnation liquid in a paint storage tank into the impregnation tank, controlling the temperature of the impregnation liquid to 80 ℃, stopping sucking the impregnation liquid when the liquid level of the impregnation liquid is 50mm higher than the top of the carbon anode plate green blank, pressurizing the impregnation tank to 0.5Mpa, and maintaining the pressure for 5 hours; taking out the raw blank of the carbon anode plate, scraping off redundant impregnation liquid on the surface of the raw blank of the carbon anode plate, and drying in the shade for 24 hours; pouring the impregnation liquid into the paint storage tank again for reuse;
step three, curing the carbon anode plate raw blank: putting the carbon anode plate raw blank processed in the step two into the impregnation tank again, boosting the pressure in the impregnation tank to 5Mpa, heating to 140-160 ℃ according to a set raw blank curing temperature-rising curve, curing for 20-30h, releasing the pressure and cooling the impregnation tank after curing is finished, and taking out the carbon anode plate raw blank; in the pressure relief process of the impregnation tank, a condensation recovery system is used for recovering and treating the discharged acetone-containing waste gas, and the acetone collected by the condensation recovery system is poured into the impregnation tank for recycling;
the raw material curing temperature rise curve is as follows: uniformly increasing the temperature from room temperature to 50 ℃ within the first 10 hours, uniformly increasing the temperature from 50 ℃ to 80 ℃ within the last 3 hours, uniformly increasing the temperature from 80 ℃ to 120 ℃ within the last 10 hours, and uniformly increasing the temperature from 120 ℃ to 150 ℃ within the last 6 hours;
the discharge port of the condensation recovery system is connected with the activated carbon adsorption system, and the condensed gas is adsorbed by activated carbon again and then discharged to the outside through the exhaust funnel; the waste active carbon is recycled after recovery treatment.
Step four, roasting the carbon anode plate green blank: placing the solidified carbon anode plate raw blanks into a well-type resistance furnace at intervals of 20-30cm for roasting, filling the adjacent carbon anode plate raw blanks with quartz sand, and roasting at the temperature of 320-380 ℃ according to a set raw blank roasting temperature rise curve; after roasting, naturally cooling the carbon anode plate to room temperature, and then using the carbon anode plate;
the green blank roasting temperature rise curve is as follows: uniformly raising the temperature from room temperature to 120 ℃ within the first 10 hours, uniformly raising the temperature from 120 ℃ to 350 ℃ within the last 10 hours, and finally keeping the temperature constant for 5 hours.
The processed carbon anode plate needs to be drilled and tapped by a lathe, a gas collecting hood and an exhaust fan are arranged above the lathe, a small amount of dust generated in the drilling and tapping processes is sucked into a water bath pool and is precipitated by a water bath, and the requirement of environmental protection is met.
Claims (6)
1. A carbon anode plate for fluorine preparation by using an impregnation method and a tail gas treatment process are characterized in that: the method comprises the following steps:
step one, processing a carbon anode plate raw blank: cutting an outsourced carbon anode plate green body according to a specified size by using a circular saw, putting the cut green body into an oven, and drying the green body for 24 hours at the temperature of 120 ℃; cooling and dedusting a saw blade of the circular saw by using water in the cutting process, and collecting the generated wastewater to a wastewater tank for precipitation and recycling;
step two, dipping the carbon anode plate raw blank: in a paint storage tank, the mass ratio of 1: 1, adding solid phenolic resin and liquid acetone in proportion to prepare impregnation liquid, neatly arranging the dried carbon anode plate green blank in an impregnation tank, preheating to 80 ℃, vacuumizing the impregnation tank to 200-500 pa, sucking the impregnation liquid in a paint storage tank into the impregnation tank, controlling the temperature of the impregnation liquid to 80 ℃, stopping sucking the impregnation liquid when the liquid level of the impregnation liquid is 50mm higher than the top of the carbon anode plate green blank, pressurizing the impregnation tank to 0.5Mpa, and maintaining the pressure for 5 hours; taking out the raw blank of the carbon anode plate, scraping off redundant impregnation liquid on the surface of the raw blank of the carbon anode plate, and drying in the shade for 24 hours; pouring the impregnation liquid into the paint storage tank again for reuse;
step three, curing the carbon anode plate raw blank: putting the carbon anode plate raw blank processed in the step two into the impregnation tank again, boosting the pressure in the impregnation tank to 5Mpa, heating to 140-160 ℃ according to a set raw blank curing temperature-rising curve, curing for 20-30h, releasing the pressure and cooling the impregnation tank after curing is finished, and taking out the carbon anode plate raw blank; in the pressure relief process of the impregnation tank, a condensation recovery system is used for recovering and treating the discharged acetone-containing waste gas, and the acetone collected by the condensation recovery system is poured into the impregnation tank for recycling;
step four, roasting the carbon anode plate green blank: placing the solidified carbon anode plate raw blanks into a well-type resistance furnace at intervals of 20-30cm for roasting, filling the adjacent carbon anode plate raw blanks with quartz sand, and roasting at the temperature of 320-380 ℃ according to a set raw blank roasting temperature rise curve; and after roasting, naturally cooling the carbon anode plate to room temperature, and then using the carbon anode plate.
2. The carbon anode plate for fluorine production and the tail gas treatment process by the impregnation method according to claim 1, wherein: and the heating mode of the oven in the first step is steam heating.
3. The carbon anode plate for fluorine production and the tail gas treatment process according to claim 1 or 2, wherein the carbon anode plate comprises: the raw material curing temperature rise curve in the third step is as follows: the temperature is increased from room temperature to 50 ℃ at a constant speed within the first 10 hours, then is increased from 50 ℃ to 80 ℃ at a constant speed within 3 hours, then is increased from 80 ℃ to 120 ℃ at a constant speed within 10 hours, and finally is increased from 120 ℃ to 150 ℃ at a constant speed within 6 hours.
4. The carbon anode plate for fluorine production and the tail gas treatment process by the impregnation method according to claim 3, wherein: the discharge port of the condensation recovery system in the third step is connected with an active carbon adsorption system, and the condensed gas is adsorbed by active carbon again and then discharged to the outside through an exhaust funnel; the waste active carbon is recycled after recovery treatment.
5. The carbon anode plate for fluorine production and the tail gas treatment process by the impregnation method according to claim 4, wherein: the green blank roasting temperature rise curve in the fourth step is as follows: uniformly raising the temperature from room temperature to 120 ℃ within the first 10 hours, uniformly raising the temperature from 120 ℃ to 350 ℃ within the last 10 hours, and finally keeping the temperature constant for 5 hours.
6. The carbon anode plate for fluorine production and the tail gas treatment process by the impregnation method according to claim 5, wherein: drilling and tapping are needed for the carbon anode plate processed in the fourth step by a lathe, a gas collecting hood and an exhaust fan are installed above the lathe, a small amount of dust generated in the drilling and tapping processes is sucked into a water bath pool, and the dust is precipitated in a water bath, so that the environment-friendly requirement is met.
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