CN109399847B - Concentration method of iron-containing waste hydrochloric acid - Google Patents
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- C02F9/00—Multistage treatment of water, waste water or sewage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01B—BOILING; BOILING APPARATUS ; EVAPORATION; EVAPORATION APPARATUS
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- B01B1/005—Evaporation for physical or chemical purposes; Evaporation apparatus therefor, e.g. evaporation of liquids for gas phase reactions
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- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
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- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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Abstract
The invention discloses a method for concentrating waste hydrochloric acid, wherein the waste hydrochloric acid is added into a blowing tower, n-hexane is vaporized through a second heat exchanger, the vaporized n-hexane is blown into the blowing tower from the bottom of the blowing tower, ammonium chloride is added into the blowing tower from a raw material tank, HCl gas, water vapor and the vaporized n-hexane escaping from a rectifying tower form mixed gas, the mixed gas enters a condensing tower, the mixed gas is condensed and liquefied and then enters a gas-liquid separator, the n-hexane condensed into liquid is heated and vaporized again and then recycled, and the non-condensed mixed gas enters a water washing tower to be absorbed by cold water to form mixed solution of n-hexane, HCl and water; and (3) separating the mixed solution in an oil-water separator, wherein n-hexane is an oil layer, the HCl aqueous solution is a water layer, and the HCl aqueous solution is discharged from a finished product tank, so that the concentration of the obtained hydrochloric acid is not lower than 21 wt%. The invention has low energy consumption, the steam in the evaporator is used for preheating the vaporized normal hexane and the waste hydrochloric acid, and the normal hexane can be recycled.
Description
Technical Field
The invention belongs to the technical field of waste liquid treatment, and particularly relates to a method for concentrating iron-containing waste hydrochloric acid.
Background
Hydrochloric acid is a common chemical product and is widely applied to carbon steel cold rolling, galvanizing and other processes. As an acid cleaning medium, hydrochloric acid reacts with iron oxide generated on the surface of steel to generate ferrous chloride and ferric chloride which are dissolved in acid liquor. The hydrochloric acid waste liquid generated by the reaction contains about 5 percent of hydrochloric acid and 10 to 12 percent of ferrous chloride and ferric chloride, and if the part of the iron-containing hydrochloric acid waste liquid is directly discharged, serious environmental pollution is caused to a discharge area. In addition, ferrous chloride and hydrogen chloride contained in the waste acid liquor are very good chemical raw materials. Therefore, the resource treatment and utilization of the iron-containing waste hydrochloric acid are necessary requirements for protecting the environment and realizing green development.
According to statistics, about 2 million tons of hydrochloric acid are needed by a push-pull pickling unit for producing 45 million tons of cold-rolled steel sheets every year, the produced hydrochloric acid-containing waste liquid is nearly 2 million tons, and the yield of the cold-rolled steel sheets in 2010 in China reaches 5100 million tons. According to the calculation, the annual production of the waste hydrochloric acid in the cold rolling industry only exceeds 220 ten thousand tons. Therefore, the resource treatment of the waste hydrochloric acid is not only environmental protection but also has very important significance for the utilization of resources and the development of improving the circular economy.
The traditional method for treating the industrial waste hydrochloric acid comprises a thermal decomposition method, a high-temperature hydrolysis method, an extraction method, a membrane separation method, a precipitation method and a neutralization method. The thermal decomposition method and the high-temperature hydrolysis method can be divided into a roasting method, a fluidized bed method and the like, the working principle of the two methods is the same, waste hydrochloric acid containing ferrous chloride reacts with oxygen at high temperature and absorbs concentrated and volatilized hydrogen chloride, and finished products of the two methods are hydrochloric acid and iron oxide red. The extraction method is to use the extraction liquid composed of organic phases for countercurrent extraction, but the method for recycling the extraction phase still has higher investment, is inconvenient to operate and is not suitable. The membrane separation method is to selectively separate iron and acid by using the ions of the membrane, and has the disadvantages that the osmotic pressure of the iron ions on two sides of the membrane is increased, so that larger pressure energy is needed to be input, the material and the pressure resistance of the membrane are required to be high, and the initial investment and the operation cost are higher. The precipitation method is to flocculate ferrous chloride in the waste hydrochloric acid by using a flocculating agent, and although part of the ferrous chloride in the waste hydrochloric acid is used, a small part of the ferrous chloride still exists in the residual waste acid liquid, so that the purity level of a product generated by the subsequent waste acid treatment is not high generally, and the performance of the product is influenced. The neutralization method adopts alkali to react with waste hydrochloric acid, which is the oldest method for treating the pickling waste liquid, but because hydrogen chloride and ferrous chloride in the waste acid liquid cannot be utilized and secondary pollution is easily caused, the method is not used at present basically.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for recycling iron-containing industrial waste hydrochloric acid, which is environment-friendly, low in investment and low in operation cost.
Therefore, the technical scheme of the invention is as follows:
1) iron-containing waste hydrochloric acid enters the stripping tower from the top of the stripping tower (3) and is sprayed downwards, n-hexane is heated and vaporized and then is blown into the stripping tower (3) from the bottom of the stripping tower, ammonium chloride enters the stripping tower (3) from the top of the stripping tower together with the waste hydrochloric acid, and part or all of hydrogen chloride in the iron-containing waste hydrochloric acid is blown out from a liquid phase to a gas phase;
in one embodiment of the invention, the temperature in the stripping tower (3) is 70-100 ℃, the concentration of the waste hydrochloric acid is 10 wt%, the waste hydrochloric acid contains 12 wt% of ferric chloride, and the ammonium chloride in the step 1): the mass ratio of the waste hydrochloric acid is (4.8-6.2): 10, the running gas speed in the stripping tower is 0.8-2.3 m/s.
2) In the stripping process, the escaped hydrogen chloride gas, normal hexane gas and water vapor enter a condensing tower (4) from the top of a stripping tower (3), wherein most of normal hexane gas is condensed into liquid and enters a gas-liquid separator (5) together with the hydrogen chloride gas and the water vapor for separation; pumping the liquid at the bottom of the stripping tower (3) into the top of the stripping tower (3) through a circulating pump (11) for circulation;
3) heating the n-hexane liquid separated in the step 2) by a reboiler (8), vaporizing again, and continuously blowing into the stripping tower for recycling; washing the uncondensed hydrogen chloride gas, the water vapor and the normal hexane gas separated in the step 2) by cold water in a washing tower (6), absorbing the water vapor and the hydrogen chloride by the cold water, and completely liquefying the normal hexane gas;
4) and the liquid absorbed by the water washing tower (6) is separated by an oil-water separator, the separated n-hexane liquid is heated and vaporized by the reboiler (8) and then enters the stripping tower (3) for recycling, and the separated water layer is discharged through a finished product tank (10).
Preferably, the bottom solution of the stripping tower (3) is pumped into a reactor (12) containing ammonium bicarbonate through a raw material pump (13) to react sufficiently to ensure that Fe contained in the waste hydrochloric acid2+、Fe3+Precipitate and ammonium chloride are generated, and solid ammonium chloride is obtained after separation, decoloration and evaporative crystallization treatment.
More preferably, the reaction in the reactor (12) is carried out under air-blast conditions, and the ferrous hydroxide in the reactor (12) is completely oxidized to ferric hydroxide.
Preferably, the precipitate and ammonium chloride generated in the reactor (12) are precipitated twice in a primary precipitation tank (15) and a secondary precipitation tank (16), and then Fe (OH) is separated3Precipitate with a small amount of dissolved Fe (OH)3The solution is fed into a bentonite precipitation tank (17), and Fe (OH) in the solution is stirred3Is absorbed by the bentonite, and the bentonite is completely separated from the solution by a third-level sedimentation tank (18).
Removal of Fe (OH)3Evaporating the water content of the solution by an evaporation crystallizer (19), and feeding the obtained solid ammonium chloride into NH4And (5) a Cl storage tank (20).
Preferably, water vapor generated during evaporation of the evaporative crystallizer (19) is used as a heat source of the reboiler (8) to supply energy for n-hexane vaporization, and the rest steam heat is used for the first heat exchanger (1) to supply energy for preheating the waste hydrochloric acid containing iron.
In the invention, the boiling point of the normal hexane is 69 ℃, the heat before vaporization is low during stripping, the industrial waste heat of 90 ℃ can be used as the heat of vaporization of the normal hexane, the dew point temperature is low during condensation, and the normal hexane can be condensed by using underground water as condensate water. And the normal hexane is insoluble in water, and the hydrogen chloride is insoluble in the normal hexane.
The invention has the following beneficial effects:
the method has low energy consumption, the vaporization heat of the normal hexane can be used as industrial waste heat, and the steam in the evaporation crystallizer is used for the vaporization of the normal hexane and the preheating of waste hydrochloric acid, so that the full utilization of energy is fully realized; the condensed water used in condensation can be underground water, is cheap and easy to obtain, does not generate toxic and harmful pollution gases, and the normal hexane can be recycled, and the iron ions in the waste acid can be treated and separated by the method.
By the concentration method, the waste hydrochloric acid with the concentration of 5-15 wt% can be concentrated to not less than 21 wt%.
Drawings
FIG. 1 is a schematic view showing the composition of an apparatus used in the method for concentrating iron-containing waste hydrochloric acid of the present invention.
In the figure:
1. first heat exchanger 2, head tank 3, blow-off tower
4. Condensing tower 5, gas-liquid separator 6 and water washing tower
7. Oil-water separator 8, reboiler 9, second heat exchanger
10. Finished product tank 11, circulating pump 12 and reactor
13. Raw material pump 14, air blower 15 and primary sedimentation tank
16. A second-stage sedimentation tank 17, a bentonite sedimentation tank 18 and a third-stage sedimentation tank
19. Evaporative crystallizer 20, ammonium chloride storage tank
Detailed Description
The method for concentrating iron-containing waste hydrochloric acid according to the present invention will be described in detail with reference to the accompanying drawings.
Referring to fig. 1, the method for concentrating iron-containing waste hydrochloric acid according to the present invention comprises the following steps:
1) iron-containing waste hydrochloric acid (dilute hydrochloric acid) enters the stripping tower from the top of the stripping tower 3 and is sprayed, normal hexane is heated and vaporized by a second heat exchanger 9 and then is blown into the stripping tower 3 from the bottom of the tower, ammonium chloride and waste hydrochloric acid enter the stripping tower 3 from the top of the tower, and part or all of hydrogen chloride in the iron-containing waste hydrochloric acid is stripped into a gas phase from a liquid phase;
in one embodiment of the present invention, the temperature in the stripping tower 3 is 70 to 100 ℃, the concentration of the waste hydrochloric acid is 10 wt%, the waste hydrochloric acid contains 12 wt% of ferric chloride, and the ratio of ammonium chloride: the mass ratio of the waste hydrochloric acid is (4.8-6.2): 10, the running gas speed in the stripping tower is 0.8-2.3 m/s.
In the step, solid ammonia chloride is added into a raw material tank 2, waste liquid in the bottom of a stripping tower 3 is pumped into the raw material tank 2 through a circulating pump 11, so that the solid ammonium chloride is dissolved, and then the mixed liquid is sprayed and circulated from the top of the stripping tower 3.
In the step, the escape rate of HCl in dilute hydrochloric acid is increased by adding n-hexane, and a small amount of water vapor is blown out together; the added ammonium chloride produces a homoionic effect which helps the hydrogen chloride to better escape from the water.
2) In the stripping process, the escaped hydrogen chloride gas, normal hexane gas and water vapor enter a condensing tower 4 from the top of a stripping tower 3, wherein most of normal hexane gas is condensed into liquid and enters a gas-liquid separator 5 together with the hydrogen chloride gas and the water vapor for separation; pumping the liquid at the bottom of the stripping tower 3 into the top of the stripping tower 3 through a circulating pump 11 for circulation;
3) heating the n-hexane liquid separated in the step 2) by a reboiler 8, vaporizing again, and continuously blowing into the stripping tower for recycling; washing the uncondensed hydrogen chloride gas, the water vapor and the normal hexane gas separated in the step 2) by cold water in a washing tower 6, absorbing the water vapor and the hydrogen chloride by the cold water, and completely liquefying the normal hexane gas;
4) the liquid after the absorption of washing tower 6 separates through oil water separator 7 (n-hexane is the oil reservoir, and the aqueous solution of hydrogen chloride is the water layer), and the n-hexane liquid of isolating passes through reboiler 8 heating vaporization back gets into stripping tower 3 recycles, and the water layer of isolating is discharged through finished product jar 10.
In the method, the bottom solution of the stripping tower 3 is pumped into a reactor 12 containing ammonium bicarbonate through a raw material pump 13 to react sufficiently so as to lead Fe contained in the waste hydrochloric acid2+、Fe3+Precipitate and ammonium chloride are generated, and solid ammonium chloride is obtained after separation, decoloration and evaporative crystallization treatment.
In order to make the reaction more complete, the reaction in the reactor 12 is carried out under continuous blowing of oxygen by the blower 14. The main reactions carried out are:
NH4HCO3+HCl→NH4Cl+H2O+CO2↑
2NH4HCO3+FeCl2→2NH4Cl+Fe(OH)2↓+2CO2↑
3NH4HCO3+FeCl3→3NH4Cl+Fe(OH)3↓+3CO2↑
4Fe(OH)2+O2+2H2O→4Fe(OH)3
the precipitate and ammonium chloride generated in the reactor 12 are precipitated twice in a primary precipitation tank 15 and a secondary precipitation tank 16 to separate Fe (OH)3Precipitate with a small amount of dissolved Fe (OH)3The solution of (A) is red-brown and is fed into a bentonite precipitation tank 17, where the Fe (OH) is present in the solution under stirring3Adsorbed by bentonite, and then completely separated from the solution by a V-105 three-stage sedimentation tank 18, the solution is colorless and transparent.
Removal of Fe (OH)3The water content of the solution is evaporated by an evaporation crystallizer 19, and the obtained solid ammonium chloride is discharged to NH4And a Cl storage tank 20 which can be used for a same ion effect agent during the purification of the hydrogen chloride.
The water vapor generated during evaporation of the evaporative crystallizer 19 is used as a heat source of the reboiler 8 to supply energy for n-hexane vaporization, and the residual steam heat is used for the first heat exchanger 1 to supply energy for waste hydrochloric acid preheating.
In the invention, the water vapor generated by the evaporative crystallizer 19 during evaporation is used as a heat source of the reboiler 8, and the residual heat of the water vapor is used for providing the preheating heat energy of the waste hydrochloric acid by the first heat exchanger 1. The preheating temperature of the waste hydrochloric acid in the prior art needs to be above 70 ℃, because the boiling point of normal hexane is 69 ℃, 90 ℃ industrial waste heat can be used as the vaporization heat of the normal hexane, the vaporized normal hexane can accelerate the escape rate of HCl in the waste hydrochloric acid, and after ammonium chloride is added, a homoionic effect is generated to help hydrogen chloride to escape from water better.
When ammonium chloride is recovered, the water vapor generated by the evaporative crystallizer 19 can be used as a heat source of a plurality of heat exchangers, on one hand, the energy is supplied for the vaporization of normal hexane, on the other hand, the energy is supplied for the preheating of waste hydrochloric acid, and the full utilization of energy is realized.
The condensed water used in the condensing tower 4 can adopt underground water, is cheap and easy to obtain, does not produce toxic and harmful pollution gases, HCl is difficult to dissolve in normal hexane, the normal hexane is insoluble in water, the normal hexane can be recycled through liquefaction and vaporization, meanwhile, the method also treats and separates out iron ions in the waste hydrochloric acid, and in addition, the ammonium chloride added from the raw material tank 2 can be recycled and reused for extracting the same-ion effect agent in the process of HCl.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (7)
1. A method for concentrating iron-containing waste hydrochloric acid is characterized by comprising the following steps:
1) iron-containing waste hydrochloric acid enters the stripping tower from the top of the stripping tower (3) and is sprayed downwards, n-hexane is heated and vaporized and then is blown into the stripping tower (3) from the bottom of the stripping tower, ammonium chloride enters the stripping tower (3) from the top of the stripping tower together with the waste hydrochloric acid, and part or all of hydrogen chloride in the iron-containing waste hydrochloric acid is blown out from a liquid phase to a gas phase;
2) in the stripping process, the escaped hydrogen chloride gas, normal hexane gas and water vapor enter a condensing tower (4) from the top of a stripping tower (3), wherein most of normal hexane gas is condensed into liquid and enters a gas-liquid separator (5) together with the hydrogen chloride gas and the water vapor for separation; pumping the liquid at the bottom of the stripping tower (3) into the top of the stripping tower (3) through a circulating pump (11) for circulation;
3) heating the n-hexane liquid separated in the step 2) by a reboiler (8), vaporizing again, and continuously blowing into the stripping tower for recycling; washing the uncondensed hydrogen chloride gas, the water vapor and the normal hexane gas separated in the step 2) by cold water in a washing tower (6), absorbing the water vapor and the hydrogen chloride by the cold water, and completely liquefying the normal hexane gas;
4) and the liquid absorbed by the water washing tower (6) is separated by an oil-water separator, the separated n-hexane liquid is heated and vaporized by the reboiler (8) and then enters the stripping tower (3) for recycling, and the separated water layer is discharged through a finished product tank (10).
2. The concentration method according to claim 1, characterized in that: the solution at the bottom of the stripping tower (3) is pumped into a reactor (12) containing ammonium bicarbonate through a raw material pump (13) to react sufficiently, so that Fe contained in the waste hydrochloric acid2+、Fe3+Precipitate and ammonium chloride are generated, and solid ammonium chloride is obtained after separation, decoloration and evaporative crystallization treatment.
3. The concentration method according to claim 2, characterized in that: the temperature in the stripping tower (3) is 70-100 ℃, the concentration of the waste hydrochloric acid is 10 wt%, the waste hydrochloric acid contains 12 wt% of ferric chloride, and the ammonium chloride in the step 1): the mass ratio of the waste hydrochloric acid is (4.8-6.2): 10, the running gas speed in the stripping tower is 0.8-2.3 m/s.
4. The concentration method according to claim 2, characterized in that: the reaction in the reactor (12) is carried out under air blast conditions, and the ferrous hydroxide in the reactor (12) is completely oxidized into ferric hydroxide.
5. The concentration method according to claim 4, characterized in that: the precipitate and ammonium chloride generated in the reactor (12) are precipitated twice in a primary sedimentation tank (15) and a secondary sedimentation tank (16) to separate Fe (OH)3Precipitate with a small amount of dissolved Fe (OH)3The solution is fed into a bentonite precipitation tank (17), and Fe (OH) in the solution is stirred3Is absorbed by the bentonite, and the bentonite is completely separated from the solution by a third-level sedimentation tank (18).
6. The concentration method according to claim 5, characterized in that: removal of Fe (OH)3Evaporating the water content of the solution by an evaporation crystallizer (19), and feeding the obtained solid ammonium chloride into NH4And (5) a Cl storage tank (20).
7. The concentration method according to claim 6, characterized in that: the water vapor generated during evaporation of the evaporative crystallizer (19) is used as a heat source of the reboiler (8) to supply energy for n-hexane vaporization, and the residual steam heat is used for the first heat exchanger (1) to supply energy for preheating the waste hydrochloric acid containing iron.
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| CN101348707A (en) * | 2007-07-19 | 2009-01-21 | 上海金发科技发展有限公司 | Rapid evaporated cooling liquid for extrudate |
| CN104495953A (en) * | 2014-12-31 | 2015-04-08 | 天津市职业大学 | Process for treating industrial waste hydrochloric acid in recycling way through salt fractionation method |
| CN107324284B (en) * | 2017-07-07 | 2020-01-14 | 天津市职业大学 | System for resourcefully handle useless hydrochloric acid of iron-containing industry |
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