CN101935077A - Waste acid concentration multistage treatment method - Google Patents
Waste acid concentration multistage treatment method Download PDFInfo
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- CN101935077A CN101935077A CN 201010266506 CN201010266506A CN101935077A CN 101935077 A CN101935077 A CN 101935077A CN 201010266506 CN201010266506 CN 201010266506 CN 201010266506 A CN201010266506 A CN 201010266506A CN 101935077 A CN101935077 A CN 101935077A
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Abstract
The invention relates to a waste acid concentration multistage treatment method which comprises the following steps of: heating 20-22% waste acid by a preheater, evaporating by a one-effect evaporation heater and a double-effect evaporation heater, cooling by a cooler and crystallizing by a crystallizer; heating by a triple-effect evaporation heater and separating by a separator to obtain 65% concentrated acid. The secondary steam part is used as a heat source part of the next stage heater and is condensed by spraying cooling water, wherein the one-effect evaporation heater and the double-effect evaporation heater are falling film graphite tube array evaporation heaters; the triple-effect evaporation heater is a floating head tube array graphite heat exchange. The water evaporation capability of the method is increased from 2.5 tons to 10 tons, and the stage number is 3 or more. A large amount of steam and cooling water is saved, and the pollution to the environment is reduced. The heat exchange area of equipment is reduced by 30%, and materials are saved and manufacturing cost is reduced correspondingly. The heat of steam is fully utilized, more than 35% of steam is saved, and more than 30% of cooling water can be saved. The condensed water part of the steam is used as the hear source part of the preheater and is recycled for other uses.
Description
Technical field
The present invention relates to a kind of low-concentration waste acid and reclaim discharge-reducing method, relate to a kind of evaporation characteristic of utilizing the body lotion vacuum flashing specifically, the moisture evaporation in the body lotion is come out, reach the method that spent acid concentrates the concentrated multiple-stage treatment of spent acid of the purpose of recycling.
Background technology
Sulfuric acid is the main raw material of Titanium White Production By Sulfuric Acid Process, has a large amount of spent acid to produce in the production process.According to the technology difference, generally the hydrolysis spent acid with concentration 17%-22% is called the vitriol oil, and 4-10% is the bleaching spent acid, generally speaking, produce the 1t finished product and can produce the 3.5t dilute sulphuric acid, wherein the 15%-20% of diluted acid total amount returns hydrolysis procedure, in order to the usefulness of the dilution vitriol oil.But traditional spent acid concentrates and exists energy consumption height, big, the concentrated back of facility investment concentration not to reach service requirements.
Zou builds the new people of grade in " ilmenite prepares the acid of titanium white by product sulfur waste and concentrates Study on reuse " " chemical industry mineral and processing ", 2005 the 3rd phases: 16 pages-18 pages, in one literary composition, point out to adopt common spent acid concentrating unit to inquire into regard to water vapour concentrating waste acid method, its equipment mainly is made up of scatterer, mist device, vaporizer, heat exchanger and vapour liquid separator.Implementation step is to squeeze into the spent acid concentrating unit after spent acid sedimentation, filtration, the slagging-off, feed water vapour and carry out heat exchange, by making mist, vapor-liquid separation, discharging carbonated drink, obtain 37% concentrated vitriol, technical process as shown in Figure 1, and point out hereof if on 37% concentrated acid basis, improve the quality mark again, can improve the spent acid reclamation rate once again, but can propose very big challenge, influence the ripening degree of equipment operation thickening equipment and concentration flow path, and will increase cost, because along with the raising of concentrated acid massfraction, the vitriolic boiling point raises rapidly, and heat energy efficiency reduces.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of spent acid concentrates multiple-stage treatment.
For solving the problems of the technologies described above, the present invention realizes like this
Spent acid concentrates the multiple-stage treatment method, comprises the steps:
Spent acid is through after the heating of I effect evaporation heater, after the separation of I effect separator, the part of liquid-state material is returned I effect evaporation heater through recycle pump, another part input II is imitated evaporation heater, after II is imitated evaporation heater and the separation of II effect separator, a part is returned II effect evaporation heater through recycle pump, another part cools off through water cooler, and crystallizer crystallization, separator separate the back filter residue to be recycled, and filtrate input III is imitated the evaporation heater heating, vapor seperator separates the back and discharges concentrated acid;
I is imitated evaporation heater and is made thermal source with saturation steam, is used to heat spent acid in the water of condensation input preheater, and the water of condensation of preheater is recycled;
III effect evaporation heater utilizes steam as thermal source, and water of condensation is recycled;
II is imitated vapor seperator and is evaporated the steam of discharging the separate chamber and do wastewater treatment after the water quench of spray condenser.
Aforesaid spent acid concentrates the multiple-stage treatment method, and described I is imitated, II effect evaporation heater is a falling liquid film graphite tubulation evaporation heater; It is tubular graphitic heat-exchanger that III is imitated evaporation heater.
Aforesaid spent acid concentrates the multiple-stage treatment method, it is characterized in that the spent acid amount in the evaporation heater reaches before the internal circulating load, material through recycle pump only at evaporation heater and vapor seperator internal recycle,
Aforesaid spent acid concentrates the multiple-stage treatment method, it is characterized in that spent acid enter I imitate evaporation heater before through the preheater preheating, the thermal source of preheater is the water of condensation that I is imitated evaporation heater.
The present invention has following positive effect:
The vaporization efficiency of falling-film evaporator is higher, and its overall heat transfer coefficient is the highest can to reach 2000Kcal/m
2H ℃, but the key of its high-efficiency evaporating is the raw water of cold conditions must be formed the layer of even fluid film at the tube interior of vaporizer, liquid distributor can be forced to form the raw water that enters vaporizer along the uniform fluid film of the ring-type of tube wall, this invention is as a Series Design, the vaporize water ability is from 2.5 tons to 10 tons, and progression is 3 grades or more.Can substitute the single-action or the double-effect evaporation technology of present widespread usage, thereby save a large amount of steam and water coolant, reduce pollution environment.
Reduce equipment heat interchanging area 30%, correspondingly saved material and reduced manufacturing cost.The heat of steam is fully used, and saves steam more than 35%, can save water coolant more than 30% simultaneously.
Description of drawings
Fig. 1 is the schema of traditional spent acid treatment process;
Fig. 2 concentrates the annexation synoptic diagram of multiple-stage treatment device for spent acid;
Fig. 3 is the structural representation of interchangeable tubular type tubulation graphite heat exchanger;
The description of symbols of major parts among Fig. 3:
A acid outlet, B show on trial, C phlegma discharging hole, the outlet of D non-condensable gases, E acid import, F steam-in, standby mouth of G, the outlet of H non-condensable gases, J condensate outlet, M, traverse baffle, K1 vapour-liquid export, the standby mouth of K2 liquidometer;
Fig. 4 is the vertical view of Fig. 3;
Fig. 5 is the structural representation of falling liquid film part;
The description of symbols of major parts among Fig. 5: 1 upper cover, 2, branch spreading liquid dish, 3, the first layer cloth liquid dish, 4, second layer cloth liquid dish, 5, graphite bolt, 6, graphite liquid-dividing head, 7, graphite grazing nut, 8, rubber seal, 10, graphite heat transfer tube, 11, graphite tube plate, 12, graphite downtake
Fig. 6 is heat transfer tube and tube sheet sealed structural representation;
The description of symbols of major parts among Fig. 6: 9, sealing graphite annulus;
Fig. 7 is cylindrical shell and tube sheet sealed structural representation;
The description of symbols of major parts among Fig. 7: 14, cylindrical shell, 16, pad.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
Fig. 2 concentrates the annexation synoptic diagram of multiple-stage treatment device for spent acid.With reference to shown in Figure 2, spent acid concentrates the multiple-stage treatment device, comprises that preheater, I are imitated evaporation heater, I is imitated between vapor seperator, II effect evaporation heater, II effect vapor seperator, water cooler, crystallizer, separator, III effect evaporation heater, vapor seperator, each parts and connected successively with pipeline.
And imitate at I that evaporation heater is imitated between the vapor seperator with I, II imitates the cyclical operation that is provided with recycle pump realization material between evaporation heater and the II effect vapor seperator; Connect recycle pump on the water cooler, water cooler is passed through in the acid that makes II imitate separator output repeatedly, strengthens cooling performance; Separator and III are imitated between the evaporation heater, I is imitated vapor seperator and imitated between the evaporation heater with II and recycle pump is set, the quick conveying of realization material.
I is imitated evaporation heater and is heated by saturated vapor, and water of condensation is delivered to preheater, as the preheater thermal source.Preheater is a piece cellular type graphite heat exchanger, and the diluted acid temperature that enters is elevated to more than 70 ℃.I is imitated the secondary steam input II effect evaporation heater that vapor seperator is discharged, for II is imitated the evaporation heater heat supply, water of condensation is done wastewater treatment after discharging, the secondary steam that II effect vapor seperator and vapor seperator are discharged is done wastewater treatment after the water quench of spray condenser, III is imitated evaporation heater by steam heating, and water of condensation is recycled.
Fig. 3 is that I, II are imitated the evaporation heater structural representation, and Fig. 4 is the vertical view of Fig. 3, and shown in Fig. 3,4, it is falling liquid film graphite tubulation evaporation heater that I, II are imitated evaporation heater, is single replace tubes formula graphite heat exchanger, and the evaporation capacity height can reach 50-80kg/m
2.h, heat interchanging area reduces more than 30% than common interchanger, and solid circulating rate reduces more than 70%.
Fig. 5 is the structural representation of falling liquid film part, with reference to shown in Figure 5, the spent acid that need be concentrated is after the sour import E input at falling liquid film graphite tubulation evaporation heater top, distribute through cloth the first layer cloth liquid dish 3, second layer cloth liquid dish 4, enter the graphite heat transfer tube 10 from graphite liquid-dividing head 6, enter separator with acid and steam behind the film forming state process graphite heat transfer tube, wherein the steam of graphite heat exchanger enters from steam-in F, export from condensate outlet behind the baffling repeatedly through traverse baffle M in the shell side, this phlegma can be used as the heating thermal source of other equipment.
Shown in Fig. 6,7, graphite heat transfer tube 10 adopt graphite products resin dedicated-modified phenolic resins passes through high pressure (500 tons of pressure) tube extruding machine extruding pipe with the Graphite Powder 99 uniform mixing, passes through high temperature (200-800 ℃) carbonizing treatment again.
Housing adopts the carbon steel line with rubber or wards off lead, guarantees its corrosion-resistant and work-ing life.
Fig. 6 is heat transfer tube and tube sheet sealed structural representation, with reference to shown in Figure 6, graphite heat transfer tube 10 adopts the sealing of single tube sealing means with tube sheet 11, connects with a cover tightness system, tightness system comprises O-ring seal 8, sealing graphite annulus 9, sealing nut 7, and O-ring seal adopts the viton material.Fig. 7 is cylindrical shell and tube sheet sealed structural representation, with reference to shown in Figure 7, reaches sealing effectiveness by pad 16 between cylindrical shell 14 and the tube sheet 11.
It is the carbon steel liner graphite-structure of two end elipse heads that I, II are imitated vapor seperator, has increased the matrix material impervious barrier between carbon steel and the graphite linings, guarantees the whole Corrosion Protection of equipment.The whole Graphite Machining Piece of external mouth of pipe liner, the intensity height, the special seal face sealing structure of design is good.Use temperature 80-180 ℃, applying pressure-0.088-0.8MPa.
The structure of graphite cooling water cooler is similar substantially to well heater, but use temperature low-15-80 ℃, applying pressure 0.2-0.4MPa.
It is tubular graphitic heat-exchanger that III is imitated graphite heater, be different from I, II effect vapor seperator part and be not to be provided with cloth liquid dish, because acid is imitated concentrating of stage through I, II, concentration nearly 60%, be easy in the equipment surface fouling, need not to adopt again the mode of falling liquid film to heat, have accessible unsteady characteristics, equipment can be worked in the very big scope of the temperature difference, can not cause damage because of expanding with heat and contract with cold of material.Use temperature is up to 220 ℃, 150 ℃ of the temperature difference.
The structure and material of vapor seperator and I, II are imitated the vapor seperator basically identical, but use temperature is higher, and erosion resistance requires higher.Use temperature 80-220 ℃, applying pressure-0.088-0.8MPa.
It is the steel lining fluorine plastics that lining is moulded recycle pump, is big flow low lift recycle pump, and not only corrosion-resistant but also high temperature resistant, watt consumption is low.
The glass reinforced plastic spray condenser is a kind of spray condensing structure, and there are four layers of tray the inside, and every layer of tray has different apertures, is staggered, and spray is even, and cooling water consumption is few, produces vacuum simultaneously.
Spent acid concentrates multilevel processing technology, comprises the steps:
Spent acid is heated to about 70 ℃ through preheater, after I is imitated the evaporation heater heating, acid and the steam of heating is imitated after separator separates through I, the part of liquid-state material is returned I effect evaporation heater through recycle pump, another part input II is imitated evaporation heater, after heating and the separation of II effect separator, a part is returned II effect evaporation heater through recycle pump, another part cools off through water cooler, the crystallizer crystallization, separator separates the back filter residue and recycles, filtrate input III is imitated the evaporation heater heating, vapor seperator separates the concentrated acid of back simmer down to 65%, and III effect evaporation heater utilizes steam as thermal source, and water of condensation is recycled.The secondary steam part is as the thermal source of next stage well heater, and the condensation of water spray partly is cooled.
Spent acid concentrates multilevel processing technology, specifically is provided with as follows:
20m
3The spent acid of concentration 20% is heated to 70 ℃-80 ℃ through preheater, input I is imitated evaporation heater, what carry in the shell side of I effect evaporation heater is the saturated steam heating, the about 120-125 of Heating temperature ℃, the about 0.25Mpa of pressure, the acid that obtains and gas-vapor mix are imitated after separator separates through I, secondary steam input II is imitated evaporation heater, spent acid is concentrated into 25% spent acid, temperature is 98-99 ℃, the part of this spent acid is returned I effect evaporation heater through recycle pump, wherein recycle pump circulation is conveyed into inventory that II imitates evaporation heater and replenishes the amount that enters I effect evaporation heater and equate substantially, to keep I to imitate the evaporation heater material balance, the spent acid input II of another is imitated and is continued heating and separating in the evaporation heater;
Imitating the evaporation heater shell side at II is that II is imitated the acidiferous secondary water vapour that separator is discharged, about 86 ℃ of temperature, the about 0.1Mpa of pressure, spent acid is after II is imitated the separator separation, secondary steam is done wastewater treatment after the water quench of spray condenser, spent acid is that concentration is about 33%, the about 68-69 of temperature ℃, and this spent acid part is imitated evaporation heater circulation heating through recycle pump input II, another part is delivered to the phase III
In the phase III, the shell side of water cooler is a refrigerated water, temperature is-6 ℃ to-10 ℃, and material inputs in the crystallizer after recycle pump circulation cooling, material is at the crystallizer intercrystalline, filter residue (main component is a ferrous sulfate) is discharged recovery after separator separates again, and filtrate is 0.3 ℃-0 ℃ of temperature, the sulfuric acid of simmer down to 40%, this filtrate is through the next stage of recycle pump input, that is:
Simmer down to concentration is 65% after III is imitated evaporation heater, vapor seperator, temperature is 99.5 ℃ the vitriol oil, and the shell side that III is imitated evaporation heater is saturated water vapour, and working temperature is 151 ℃, and pressure is 0.4Mpa, and water of condensation is recycled.Material obtains about 10m after evaporation separates
3Temperature is 99.5-100.5 ℃, and concentration is 65% concentrated acid, and steam is done wastewater treatment after the spray condenser cooling.
The application cycle pump is back to evaporation heater with partial material, and another part material enters the explanation in next stage, and the material in evaporation heater reaches internal circulating load (about 150m
3) before, material, reaches after the internal circulating load in the heating of evaporation heater internal recycle through recycle pump, partial material can enter the next stage.The working condition of the recycle pump that connects on the water cooler is identical therewith, and the material in water cooler reaches before the internal circulating load, and recycle pump passes through water cooler with material repeatedly.
I, II, III are imitated the technical characteristic of operation stage, water cooler shown in table 1, table 2, table 3, table 4.
Table 1 is the list of technical characteristics that I is imitated the stage:
Table 2 is lists of technical characteristics that II is imitated:
Table 3 be water cooler list of technical characteristics:
Table 4 is lists of technical characteristics that III is imitated:
Above-mentioned embodiment does not limit technical scheme of the present invention in any form, and the technical scheme that mode obtained that every employing is equal to replacement or equivalent transformation all drops on protection scope of the present invention.
Claims (4)
1. spent acid concentrates the multiple-stage treatment method, it is characterized in that comprising the steps:
Spent acid is through after the heating of I effect evaporation heater, after the separation of I effect separator, the part of liquid-state material is returned I effect evaporation heater through recycle pump, another part input II is imitated evaporation heater, after II is imitated evaporation heater and the separation of II effect separator, a part is returned II effect evaporation heater through recycle pump, another part cools off through water cooler, and crystallizer crystallization, separator separate the back filter residue to be recycled, and filtrate input III is imitated the evaporation heater heating, vapor seperator separates the back and discharges concentrated acid;
I is imitated evaporation heater and is made thermal source with saturation steam, and water of condensation is recycled, as the thermal source of preheater;
II is imitated vapor seperator and is evaporated the secondary steam of discharging the separate chamber and do wastewater treatment after the water quench of spray condenser;
III effect evaporation heater utilizes steam as thermal source, and water of condensation is recycled.
2. spent acid according to claim 1 concentrates the multiple-stage treatment method, it is characterized in that described I is imitated, II effect evaporation heater is a falling liquid film graphite tubulation evaporation heater; It is tubular graphitic heat-exchanger that III is imitated evaporation heater.
3. spent acid according to claim 1 concentrates the multiple-stage treatment method, it is characterized in that the spent acid amount in the evaporation heater reaches before the internal circulating load, material through recycle pump only at evaporation heater and vapor seperator internal recycle,
4. spent acid according to claim 1 concentrates the multiple-stage treatment method, it is characterized in that spent acid enter I imitate evaporation heater before through the preheater preheating, the thermal source of preheater is the water of condensation that I is imitated evaporation heater.
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| CN102249203A (en) * | 2011-04-29 | 2011-11-23 | 南通京通石墨设备有限公司 | Phosphoric acid evaporation process and device thereof |
| CN102633238A (en) * | 2012-04-12 | 2012-08-15 | 中国科学院过程工程研究所 | Process method of concentrating and purifying dilute sulphuric acid |
| CN102730650A (en) * | 2011-04-12 | 2012-10-17 | 安徽理工大学 | Recovery technology of titanium white waste acid |
| CN102774816A (en) * | 2012-08-02 | 2012-11-14 | 潜江方圆钛白有限公司 | Method and device for concentrating waste acid in titanium dioxide production by sulfuric acid process |
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| CN105399168A (en) * | 2015-12-18 | 2016-03-16 | 许达人 | Multi-effect evaporation and concentration device and technology thereof for solution containing sulfuric acid and salts thereof |
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| CN102633238A (en) * | 2012-04-12 | 2012-08-15 | 中国科学院过程工程研究所 | Process method of concentrating and purifying dilute sulphuric acid |
| CN102633238B (en) * | 2012-04-12 | 2014-09-24 | 中国科学院过程工程研究所 | Process method of concentrating and purifying dilute sulphuric acid |
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