CN105731394A - Refined sulfuric acid preparation device and preparation method thereof - Google Patents
Refined sulfuric acid preparation device and preparation method thereof Download PDFInfo
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- CN105731394A CN105731394A CN201511014178.2A CN201511014178A CN105731394A CN 105731394 A CN105731394 A CN 105731394A CN 201511014178 A CN201511014178 A CN 201511014178A CN 105731394 A CN105731394 A CN 105731394A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
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Abstract
The invention discloses a refined sulfuric acid preparation device and a preparation method thereof. The preparation device comprises a fuming sulfuric acid washing tower, a refined sulfuric acid absorption tower, a flue gas filter, a concentrated acid cooler, an absorption tower circulation acid pump, an absorption tower acid cooler, a refined acid circulation groove, a degassing tower, and a finished acid storage tank. On the basis of a conventional sulfuric acid device, a refined sulfuric acid device and a preparation method are constructed to cooperate with the conventional sulfuric acid device so as to produce refined sulfuric acid products. An air exhaust absorption method is adopted, flue gas is taken as the raw material and is directly absorbed by refined sulfuric acid; the purity of finished product is high, the production efficiency is high, and the conversion cost is low. The wastes are smartly converted into valuable resources, the environment is protected, the resources are maximally utilized, and thus the device and method are worthy to popularize.
Description
Technical field
The present invention relates to sulphuric acid preparation field, particularly relate to a kind of POV preparation facilities and preparation method.
Background technology
In existing antacid field, the sulfuric acid product that smelting lead sulphuric acid plant is made is adopted mostly to be the industrial sulphuric acid of purity about 98%, but containing impurity inside the sulphuric acid of technical grade, and its purity is uncertain, the inside is likely to there is heavy metal, ash, chlorine, sulfur dioxide etc., industrial sulphuric acid is used for the refining of oil, the smelting of non-ferrous metal, the pickling processes of iron and steel, leather making process and coking industry, the fields such as light textile industry, but for the field that sulphuric acid purity requirement is higher, such as: accumulator raw material, medicine and other fields, and be specifically used to and do chemical experiment, the reagent of sulfuric acid that chemical analysis uses, require very high purity, impurity content is almost nil.Obvious industrial sulphuric acid can not meet the market demand, it is necessary to the POV that industrial sulphuric acid is finer relatively.But, adopt traditional smelting lead sulphuric acid plant also not possess at present and prepare POV function, POV of the prior art preparation exists device complexity more, technique is loaded down with trivial details, production efficiency is low, and annual production is low, and end product quality such as is difficult to control at the problems.
Summary of the invention
It is an object of the invention to overcome the technical problem that in prior art, smelting lead sulphuric acid plant exists, on the basis of smelting lead sulphuric acid plant, a set of POV preparation facilities and a kind of new POV preparation method are provided, this covering device can make POV, production yields is high, production efficiency is fast, converts cost low, and finished product purity is high.
nullTechnical scheme: a kind of POV preparation facilities，Including oleum scrubbing tower、POV absorption tower、Smoke filter、Concentrated acid cooler、Absorption tower cyclic acid pump、Absorption tower acid cooler、Refining acid circulating slot、Degassing tower、Finished acid basin，Described oleum scrubbing tower import connects heat exchanger POV exhanst gas outlet，The outlet of oleum scrubbing tower connects smoke filter import，The outlet of described smoke filter connects the import of POV absorption tower，Concentrated acid outlet is set bottom POV absorption tower，The outlet of described concentrated acid connects concentrated acid cooler by the road，Concentrated acid cooler outlet connects refining acid circulating slot，It is communicated with pure water inlet pipeline in described refining acid circulating slot，Described refining acid circulating slot outlet sprays inlet communication again through absorption tower acid cooler and POV absorption tower，Again spray in refining acid circulating slot outlet and POV absorption tower pipeline is provided with between import absorption tower cyclic acid pump，The outlet of described POV adsorption tower smoke is connected transducer after converging with the main pipeline of the first absorption tower outlet，Industrial sulphuric acid process units is connected by transducer，Described POV absorption tower POV certified products discharging opening connects degassing tower by the road，Described degassing tower discharging opening connects finished acid basin through finished product transfer pipeline，And finished acid cooler and finished acid pump are installed on finished product transfer pipeline.
Based on technique scheme, it is connected to air filter and air blower at degassing tower air inlet.
Based on technique scheme, being connected a dosing tank with degassing tower side, described dosing tank is connected to oxidant gravitation tank.
A kind of POV preparation method adopting above-mentioned preparation facilities, the method comprises the following steps:
Step one, after sulfur dioxide flue gas converted device first time conversion, by Valve controlling, wherein the flue gas of 60～75% directly goes to the first absorption tower to produce technical grade sulphuric acid, and the flue gas of 25～40% enters POV preparation facilities；
nullStep 2，The flue gas containing SO3 entering POV preparation facilities initially enters the washing of oleum scrubbing tower，Remove the impurity in flue gas，Flue gas after washing enters in smoke filter refining，Flue gas after exquisiteness enters back into POV absorption tower，By temperature 60～75 DEG C、Concentration is the POV spray of 98.1%～98.5%，To absorb the SO3 in gas，Wherein absorbance is more than 99.4%，In absorption gas, the sulphuric acid after SO3 goes out from tower underflow、Refining acid circulating slot is entered after concentrated acid cooler cools down，Refining acid circulating slot adds pure water，Adjust sulfuric acid concentration to normal acid dense 98～98.5%，Absorption tower acid cooler is sent into by absorption tower cyclic acid pump，Cool down through recirculated cooling water in the acid cooler of absorption tower，Sulphuric acid temperature is made to be cooled to less than 60 degree，Then enter back into POV absorption tower and adopt the spray acid spray-absorption again of 95～98%，To absorb the sulfur dioxide dissolved in sulphuric acid，According to analytical pure exquisiteness sulphuric acid index，The exquisite sulphuric acid that output is qualified；
Step 3, absorbs SO through POV absorption tower3After flue gas export from POV absorption tower after, then converge with the main pipeline of the first absorption tower outlet, the common converter that enters carries out twice transformation and produces industrial sulphuric acid；
Step 4, sends into degassing tower elimination SO by purified grade sulphuric acid qualified for output in step 22Gas, removes SO2It is cooled to room temperature after gas, is pumped up into fill head tank, carry out entrucking or tinning then through putting acid tube.
Based on technique scheme, in described step 2, in refining acid circulating slot, added pure water is that the pure water that boiler desalted water produces with first-stage reverse osmosis device mixes, and mixed proportion is: 1:1.
Based on technique scheme, in described step 4, degassing tower adopts that to blast air method degassed, and the air blasted is filtered cleaned air.
Beneficial effects of the present invention: the present invention applies for artificially increasing product variety, meeting the market requirement, improves Business Economic Benefit, on the basis of existing sulfuric acid apparatus, and a set of POV device of auxiliary construction and preparation method.Particularly as follows: adopt the direct absorption process of flue gas to produce the technology of POV product, a set of POV device of auxiliary construction on existing annual production smelting lead sulphuric acid plant, sulfur trioxide derive from that smelting lead sulphuric acid plant first time converts out containing SO3Flue gas.Finished product purity is high, and production efficiency is fast, converts cost low, cleverly garbage is turned waste into wealth, both solved environmental issue, maximized again make use of existing resource, suitable production in enormous quantities, production efficiency is high, and product quality is easily controlled, added pure water is through membrane filtration, the water quality of output is stable, it is easy to controlling, quality is good, benefiting the nation and the people, this covering device is in the highly promotion and implementation of antacid field.
Figure of description
Fig. 1 is POV preparation facilities process chart of the present invention.
Number in the figure: 1-transducer, 2-oleum scrubbing tower, 3-smoke filter, 4-POV absorption tower, 5-concentrated acid cooler；6-refining acid circulating slot, 7-absorption tower cyclic acid pump, 8-pure water inlet pipeline, 9-absorption tower acid cooler, 10-degassing tower, 11-finished acid cooler, 12-finished acid pump, 13-finished acid basin, 14-the first absorption tower, 15-industrial sulphuric acid process units.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described, in order to is better understood from technical solution of the present invention.
Embodiment 1: the POV preparation facilities of the present embodiment, it is on the basis that existing a set of 120,000 tons/year of smelting lead sulphuric acid plants, product are 98% industrial sulphuric acid, for increasing product variety, meeting the market requirement, the a set of POV preparation facilities of auxiliary construction, POV preparation facilities annual gas is dense presses 8% for this, enters to convert tolerance 49108Nm3/h, scale design is for producing 30000 tons per year, and sulphuric acid prescription reaches analytical pure (AR level).Require that this maximum productivity is 40,000 tons.Specific as follows:
Referring to Fig. 1, including oleum scrubbing tower 2, POV absorption tower 4, smoke filter 3, concentrated acid cooler 5, absorption tower cyclic acid pump 7, absorption tower acid cooler 9, refining acid circulating slot 6, degassing tower 10, finished acid basin 13, described oleum scrubbing tower import connects heat exchanger POV exhanst gas outlet, the outlet of oleum scrubbing tower connects smoke filter import, the outlet of described smoke filter connects the import of POV absorption tower, wherein smoke filter adopts high efficiency particulate air filter, and filter element adopts glass fiber winding.This smoke filter can dedusting deironing, original acid foam and acid mist can be removed again.Guarantee flue gas cleaning free from admixture.nullConcentrated acid outlet is set bottom POV absorption tower，The outlet of described concentrated acid connects concentrated acid cooler by the road，Concentrated acid cooler outlet connects refining acid circulating slot，It is communicated with pure water inlet pipeline in described refining acid circulating slot，Described refining acid circulating slot outlet sprays inlet communication again through absorption tower acid cooler and POV absorption tower，Again spray in refining acid circulating slot outlet and POV absorption tower pipeline is provided with between import absorption tower cyclic acid pump，The outlet of described POV adsorption tower smoke is connected transducer after converging with the main pipeline of the first absorption tower outlet，Industrial sulphuric acid process units is connected by transducer，Described POV absorption tower POV certified products discharging opening connects degassing tower by the road，Described degassing tower discharging opening connects finished acid basin through finished product transfer pipeline，And finished acid cooler and finished acid pump are installed on finished product transfer pipeline，In this enforcement, acid pump all adopts fluoroplastic pump.
The present embodiment adopts the method that above-mentioned preparation facilities prepares POV, process chart shown in Figure 1, specific as follows:
Step one, sulfur dioxide flue gas converted device first time arranges a bypass duct after converting before entering a suction tower, and by Valve controlling, wherein the flue gas of 70% directly goes to the first absorption tower to produce technical grade sulphuric acid, and the flue gas of 30% enters POV preparation facilities；
Step 2, the flue gas containing SO3 entering POV preparation facilities initially enters the washing of oleum scrubbing tower, impurity in flue gas is washed, impurity is made to enter in oleum, oleum decomposites SO3 gas, flue gas after washing enters in smoke filter refining, through smoke filter, contaminant filters such as iron content, SO3 is made to become purer, flue gas after exquisiteness enters back into POV absorption tower, with temperature 70 C, concentration is the POV spray of 98.3%, to absorb the SO3 in gas, wherein absorbance is more than 99.4%, in absorption gas, the sulphuric acid after SO3 goes out from tower underflow, refining acid circulating slot is entered after the cooling of cooled device, sulphuric acid after the cooling of cooled device enters the inlet temperature of refining acid circulating slot and controls less than 60 degree.nullRefining acid circulating slot adds pure water，Adjust sulfuric acid concentration to normal acid dense 98.2%，Absorption tower acid cooler is sent into by absorption tower cyclic acid pump，Cool down through recirculated cooling water in the acid cooler of absorption tower，Sulphuric acid temperature is made to be cooled to less than 60 degree，Then enter back into POV absorption tower and adopt the spray acid spray-absorption again of concentration 97%，To absorb the sulfur dioxide dissolved in sulphuric acid，According to analytical pure exquisiteness sulphuric acid index，The exquisite sulphuric acid that output is qualified，Qualified POV standard is GB625/T-2007 analytical reagent sulphuric acid index，Shown in table one，This step adopts absorption process of bleeding，The Technology directly absorbed with POV，Wherein: in refining acid circulating slot, added pure water is that the pure water that boiler desalted water produces with first-stage reverse osmosis device mixes，Mixed proportion is: 1:1；
Step 3, absorbs SO through POV absorption tower3After flue gas export from POV absorption tower after, then converge with the main pipeline of the first absorption tower outlet, the common converter that enters carries out twice transformation and produces industrial sulphuric acid；
Step 4, sends into degassing tower elimination SO by purified grade sulphuric acid qualified for output in step 22Gas, removes SO2POV after gas is cooled to room temperature, is pumped up into fill head tank, carries out entrucking or tinning then through putting acid tube, it is degassed that degassing tower adopts employing to blast air method, air used is filtered cleaned air, degassing tower expellant gas, imports two suction tower outlets.
Embodiment 2: the preparation method of a kind of POV, process chart shown in Figure 1, specific as follows:
Step one, sulfur dioxide flue gas converted device first time arranges a bypass duct after converting before entering a suction tower, and by Valve controlling, wherein the flue gas of 60% directly goes to the first absorption tower to produce technical grade sulphuric acid, and the flue gas of 40% enters POV preparation facilities；
Step 2, the flue gas containing SO3 entering POV preparation facilities initially enters the washing of oleum scrubbing tower, impurity in flue gas is washed, impurity is made to enter in oleum, oleum decomposites SO3 gas, flue gas after washing enters in smoke filter refining, through smoke filter, contaminant filters such as iron content, SO3 is made to become purer, flue gas after exquisiteness enters back into POV absorption tower, with temperature 60 C, concentration is the POV spray of 98.1%, to absorb the SO3 in gas, wherein absorbance is more than 99.4%, in absorption gas, the sulphuric acid after SO3 goes out from tower underflow, refining acid circulating slot is entered after concentrated acid cooler cools down, wherein, sulphuric acid after concentrated acid cooler cools down enters the inlet temperature of refining acid circulating slot and controls less than 60 degree.Refining acid circulating slot adds pure water, adjust sulfuric acid concentration to normal acid dense 98%, absorption tower acid cooler is sent into by absorption tower cyclic acid pump, cool down through recirculated cooling water in the acid cooler of absorption tower, sulphuric acid temperature is made to be cooled to less than 60 degree, then enter back into POV absorption tower and adopt the spray acid spray-absorption again of concentration 95%, to absorb the sulfur dioxide dissolved in sulphuric acid, according to analytical pure exquisiteness sulphuric acid index, the exquisite sulphuric acid that output is qualified, qualified POV standard is GB625/T-2007 analytical reagent sulphuric acid index, shown in table one；
Step 3, absorbs SO through POV absorption tower3After flue gas export from POV absorption tower after, then converge with the main pipeline of the first absorption tower outlet, the common converter that enters carries out twice transformation and produces industrial sulphuric acid；
Step 4, sends into degassing tower elimination SO by purified grade sulphuric acid qualified for output in step 22Gas, removes SO2POV after gas is cooled to room temperature, is pumped up into fill head tank, carries out entrucking or tinning then through putting acid tube, and degassing tower adopts filtered cleaned air, degassing tower expellant gas, imports two suction tower outlets.
Embodiment 3: the preparation method of a kind of POV, process chart shown in Figure 1, specific as follows:
Step one, sulfur dioxide flue gas converted device first time arranges a bypass duct after converting before entering a suction tower, and by Valve controlling, wherein the flue gas of 75% directly goes to the first absorption tower to produce technical grade sulphuric acid, and the flue gas of 25% enters POV preparation facilities；
Step 2, the flue gas containing SO3 entering POV preparation facilities initially enters the washing of oleum scrubbing tower, impurity in flue gas is washed, impurity is made to enter in oleum, oleum decomposites SO3 gas, flue gas after washing enters in smoke filter refining, through smoke filter, contaminant filters such as iron content, SO3 is made to become purer, flue gas after exquisiteness enters back into POV absorption tower, by temperature 75 DEG C, concentration is the POV spray of 98.5%, to absorb the SO3 in gas, wherein absorbance is more than 99.4%, in absorption gas, the sulphuric acid after SO3 goes out from tower underflow, refining acid circulating slot is entered after concentrated acid cooler cools down, wherein, sulphuric acid after concentrated acid cooler cools down enters the inlet temperature of refining acid circulating slot and controls less than 60 degree.Refining acid circulating slot adds pure water, adjust sulfuric acid concentration to normal acid dense 98.5%, absorption tower acid cooler is sent into by absorption tower cyclic acid pump, cool down through recirculated cooling water in the acid cooler of absorption tower, sulphuric acid temperature is made to be cooled to less than 60 degree, then enter back into POV absorption tower and adopt the spray acid spray-absorption again of concentration 98%, to absorb the sulfur dioxide dissolved in sulphuric acid, according to analytical pure exquisiteness sulphuric acid index, the exquisite sulphuric acid that output is qualified, qualified POV standard is GB625/T-2007 analytical reagent sulphuric acid index, shown in table one；
Step 3, absorbs SO through POV absorption tower3After flue gas export from POV absorption tower after, then converge with the main pipeline of the first absorption tower outlet, the common converter that enters carries out twice transformation and produces industrial sulphuric acid；
Step 4, sends into degassing tower elimination SO by purified grade sulphuric acid qualified for output in step 22Gas, removes SO2POV after gas is cooled to room temperature, is pumped up into fill head tank, carries out entrucking or tinning then through putting acid tube, and degassing tower adopts filtered cleaned air, degassing tower expellant gas, imports two suction tower outlets.
Table one:
| Project | Analytical pure POV index GB/T 625-2007 |
| H2SO4 | 95~98% |
| Free sulfur trioxide (SO3) content | -- |
| Ash | ≤ 0.001% |
| Fe | ≤0.00005% |
| As | ≤0.000003% |
| Hg | |
| Cu | ≤0.00001% |
| Pb | ≤0.00001% |
| Chloride (Cl) | ≤ 0.00003% |
| Nitrate (NO3) | ≤ 0.00005% |
| Ammonium salt (NH4) | ≤0.0002% |
| Transparency | |
| Color Degree, black Zeng Danwei | ≤10 |
| Potassium permanganate reducing substances (SO2) | ≤ 0.0005% |
| Ignition residue (in sulfate) w/% | ≤0.001% |
Claims (6)
- null1. a POV preparation facilities，It is characterized in that: include oleum scrubbing tower、POV absorption tower、Smoke filter、Concentrated acid cooler、Absorption tower cyclic acid pump、Absorption tower acid cooler、Refining acid circulating slot、Degassing tower and finished acid basin，Described oleum scrubbing tower import connects heat exchanger POV exhanst gas outlet，The outlet of oleum scrubbing tower connects smoke filter import，The outlet of described smoke filter connects the import of POV absorption tower，Concentrated acid outlet is set bottom POV absorption tower，The outlet of described concentrated acid connects concentrated acid cooler by the road，Concentrated acid cooler outlet connects refining acid circulating slot，It is communicated with pure water inlet pipeline in described refining acid circulating slot，Described refining acid circulating slot outlet sprays inlet communication again through absorption tower acid cooler and POV absorption tower，Again spray in refining acid circulating slot outlet and POV absorption tower pipeline is provided with between import absorption tower cyclic acid pump，The outlet of described POV adsorption tower smoke is connected transducer after converging with the main pipeline of the first absorption tower outlet，Industrial sulphuric acid process units is connected by transducer，Described POV absorption tower POV certified products discharging opening connects degassing tower by the road，Described degassing tower discharging opening connects finished acid basin through finished product transfer pipeline，And finished acid cooler and finished acid pump are installed on finished product transfer pipeline.
- 2. POV preparation facilities according to claim 1, is characterized in that: be connected to air filter and air blower at degassing tower air inlet.
- 3. POV preparation facilities according to claim 1, is characterized in that: be connected a dosing tank with degassing tower side, described dosing tank is connected to oxidant gravitation tank.
- 4. adopt a POV preparation method for preparation facilities as claimed in claim 1, it is characterized in that: the method comprises the following steps:Step one, after sulfur dioxide flue gas converted device first time conversion, by Valve controlling, wherein the flue gas of 60～75% directly goes to the first absorption tower to produce technical grade sulphuric acid, and the flue gas of 25～40% enters POV preparation facilities；nullStep 2，The flue gas containing SO3 entering POV preparation facilities initially enters the washing of oleum scrubbing tower，Remove the impurity in flue gas，Flue gas after washing enters in smoke filter refining，Flue gas after exquisiteness enters back into POV absorption tower，By temperature 60～75 DEG C、Concentration is the POV spray of 98.1%～98.5%，To absorb the SO3 in gas，Wherein absorbance is more than 99.4%，In absorption gas, the sulphuric acid after SO3 goes out from tower underflow、Refining acid circulating slot is entered after concentrated acid cooler cools down，Refining acid circulating slot adds pure water，Adjust sulfuric acid concentration to normal acid dense 98～98.5%，Absorption tower acid cooler is sent into by absorption tower cyclic acid pump，Cool down through recirculated cooling water in the acid cooler of absorption tower，Sulphuric acid temperature is made to be cooled to less than 60 degree，Then enter back into POV absorption tower and adopt the spray acid spray-absorption again of concentration 95～98%，To absorb the sulfur dioxide dissolved in sulphuric acid，According to analytical pure exquisiteness sulphuric acid index，The exquisite sulphuric acid that output is qualified；Step 3, absorbs SO through POV absorption tower3After flue gas export from POV absorption tower after, then converge with the main pipeline of the first absorption tower outlet, the common converter that enters carries out twice transformation and produces industrial sulphuric acid；Step 4, sends into degassing tower elimination SO by purified grade sulphuric acid qualified for output in step 22Gas, removes SO2It is cooled to room temperature after gas, is pumped up into fill head tank, carry out entrucking or tinning then through putting acid tube.
- 5. POV preparation method according to claim 4, is characterized in that: in described step 2, in refining acid circulating slot, added pure water is that the pure water that boiler desalted water produces with first-stage reverse osmosis device mixes, and mixed proportion is: 1:1.
- 6. POV preparation method according to claim 4, is characterized in that: in described step 4, degassing tower adopts that to blast air method degassed, and the air blasted is filtered cleaned air.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106422680A (en) * | 2016-11-22 | 2017-02-22 | 杭州东日节能技术有限公司 | Smelting off-gas purification treatment device and method capable of producing by-product sulfuric acid with the concentration being 40% or higher |
| CN109336065A (en) * | 2018-11-20 | 2019-02-15 | 惠州市百利宏晟安化工有限公司 | A kind of manufacturing method of high purity extractive Sulphuric acid |
| CN109879255A (en) * | 2019-04-27 | 2019-06-14 | 招远市招金金合科技有限公司 | A kind of system and method for pyrite-based sulfuric acid production system production refined sulfuric acid |
| CN112452108A (en) * | 2020-12-30 | 2021-03-09 | 双盾环境科技有限公司 | By using a gas containing SO3Method for increasing concentration of conventional concentration sulfuric acid in dry flue gas |
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Application publication date: 20160706 |