CN110589779A - Sulfuric acid system production liquid SO3Practical and safe process - Google Patents
Sulfuric acid system production liquid SO3Practical and safe process Download PDFInfo
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- CN110589779A CN110589779A CN201911060661.2A CN201911060661A CN110589779A CN 110589779 A CN110589779 A CN 110589779A CN 201911060661 A CN201911060661 A CN 201911060661A CN 110589779 A CN110589779 A CN 110589779A
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- sulfuric acid
- fuming sulfuric
- liquid
- water
- evaporator
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000007788 liquid Substances 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 69
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 claims abstract description 91
- 239000007789 gas Substances 0.000 claims abstract description 49
- 238000001704 evaporation Methods 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 239000003546 flue gas Substances 0.000 claims abstract description 23
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003860 storage Methods 0.000 claims abstract description 19
- 230000008020 evaporation Effects 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 89
- 239000002253 acid Substances 0.000 claims description 52
- 238000010521 absorption reaction Methods 0.000 claims description 37
- 230000004087 circulation Effects 0.000 claims description 18
- 238000001556 precipitation Methods 0.000 claims description 11
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 230000026676 system process Effects 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 238000009833 condensation Methods 0.000 abstract description 11
- 230000005494 condensation Effects 0.000 abstract description 11
- 238000004064 recycling Methods 0.000 abstract description 5
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Inorganic materials O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 107
- 239000000047 product Substances 0.000 description 16
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000000779 smoke Substances 0.000 description 6
- 125000004122 cyclic group Chemical group 0.000 description 4
- 229960003512 nicotinic acid Drugs 0.000 description 4
- 235000001968 nicotinic acid Nutrition 0.000 description 4
- 239000011664 nicotinic acid Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 239000013589 supplement Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- -1 sodium alkyl benzene Chemical class 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
- C01B17/74—Preparation
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention discloses a sulfuric acid system for producing liquid SO3The practical and safe process comprises the following steps: process 1, passing the dry hot flue gas through SO3In the evaporator, is SO3The evaporator provides evaporation heat; 2, fully preheating and heating the fuming sulfuric acid solution by the spiral plate type preheater, and conveying the fuming sulfuric acid solution to SO3The evaporator is heated to carry out SO3Evaporating, wherein the evaporated high-temperature fuming sulfuric acid solution with reduced concentration passes through a spiral plate type preheater, fully preheating the concentrated fuming sulfuric acid to be evaporated, and flowing back to the fuming sulfuric acid circulating tank after cooling; process 3, SO3The evaporator is heated to evaporate fuming sulfuric acid and separate pure SO3Introducing the gas into a double-row micro-slope sprinkling-falling type condenser for condensation treatment, and condensing the gas into SO3Liquid, flowing into liquid SO3And (5) obtaining a product by the finished product storage tank. Production of liquid SO according to the invention3The practical and safe process fully and efficiently realizes the utilization of system heatAnd the recycling is realized, the production cost is greatly reduced, the reliability and the safety are improved, and the problems of insufficient evaporation heat and the safety and the high efficiency of the condenser are effectively solved.
Description
Technical Field
The invention relates to the technical field of sulfuric acid production, in particular to a method for producing liquid SO by a sulfuric acid system3The practical and safe process.
Background
Liquid SO3Mainly used as a sulfonating agent, which is an intermediate product for preparing high-concentration fuming sulfuric acid and chlorosulfonic acid. At present, a large amount of domestic sulfur trioxide is used for preparing sodium alkyl benzene sulfonate, sulfonated lubricating oil for preparing white oil, biological pharmacy and the like. The high-concentration oleum is mainly used as a sulfonating agent, a smoke bomb and the like for sulfonation reaction. SO (SO)3The liquid has strong volatility, is easy to freeze, cannot meet water and belongs to dangerous chemicals, so the production safety is very important.
The existing production method mainly has three problems: firstly, the heat required by evaporation is often insufficient, the evaporation and the yield are influenced, some steam heating with the pressure of about 0.8MPa has to be adopted, and the energy consumption also brings risks; secondly, the condensation capacity is small and restricted, the cooling water is large or is cooled, so that the solidification and blockage are easy to occur, and the treatment is very troublesome; cooling water is low or heat yield is affected, SO3The gas is influenced by the condensation speed, the amount of the gas entering the condenser is limited, the gas cannot directly pass through the condenser and must be condensed; the third is that the condenser takes high-efficiency cooling and safety into consideration, and no good method exists, namely, high water cooling effect is needed, water leakage is feared to cause accidents, and air cooling is often adopted for safety, so that the efficiency is extremely low, and the effect is particularly obvious in summer.
Disclosure of Invention
The present invention is proposed to solve the above problems in the prior artSulfuric acid system production liquid SO3The practical and safe process.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a sulfuric acid system for producing liquid SO3The practical and safe process comprises the following steps:
in the process 1, dry hot flue gas generated by the sulfuric acid system process passes through SO3In the evaporator, is SO3The evaporator provides evaporation heat;
2, fully preheating and heating the fuming sulfuric acid solution by the spiral plate type preheater, and conveying the fuming sulfuric acid solution to SO3The evaporator is heated to carry out SO3Evaporating, and discharging SO from high-temperature fuming sulfuric acid solution with reduced concentration after evaporation3The evaporator returns to pass through the spiral plate type preheater, fully preheats concentrated fuming sulfuric acid to be evaporated, and flows back to the fuming sulfuric acid circulating tank after being cooled;
process 3, SO3The evaporator is heated to evaporate fuming sulfuric acid and separate pure SO3Introducing the gas into a double-row micro-slope shower-falling type condenser for condensation treatment, wherein all or most of SO3The gas is condensed into SO3Liquid, flowing into liquid SO3The finished product is stored in a storage tank to obtain a product without condensed SO3The gas enters fuming sulfuric acid SO3And an acid return pipe of the absorption tower.
Further, the sulfuric acid system produces liquid SO3The practical and safe process specifically comprises the following steps:
in the process 1, hot flue gas generated by the sulfuric acid system process passes through SO3In the evaporator, is the SO3The evaporator provides heat of vaporization via the SO3Fuming sulfuric acid SO is introduced into the flue gas after heat exchange and temperature reduction of the evaporator3In the absorption tower;
step 2, pumping fuming sulfuric acid liquid in a fuming sulfuric acid circulating tank out by a circulating pump to be circulated in two ways, wherein the first way is conveyed to a spiral plate type cooler for cooling treatment, and the other way is conveyed to a spiral plate type preheater for heating treatment; specifically, the method comprises the following steps:
the first path is conveyed to the fuming sulfuric acid solution cooled by the spiral plate coolerSulfuric acid SO of flue gas3An absorption tower for absorbing the introduced fuming sulfuric acid SO3SO contained in flue gas in absorption tower3Returning the obtained high-concentration oleum to the oleum circulating tank to supplement SO of oleum liquid3Content (c);
the second path of fuming acid liquor preheated and heated by the spiral plate type preheater is conveyed to SO3The evaporator is used for evaporating and separating out pure SO3Gas, high temperature oleum with reduced concentration after evaporation3The evaporator returns to the fuming sulfuric acid circulating tank through the spiral plate type preheater;
and 3, process: SO (SO)3Pure SO is separated from fuming sulfuric acid by evaporation of an evaporator3Introducing the gas into a double-row micro-slope shower-falling type condenser for cooling treatment, wherein all or most of SO3The gas is condensed into SO3Liquid, flowing into liquid SO3The finished product is stored in a storage tank to obtain a product; without condensed SO3The gas enters fuming sulfuric acid SO3And dissolving the mixture into fuming sulfuric acid solution in an acid return pipe of the absorption tower, and allowing the mixture to enter a fuming sulfuric acid circulating tank for recycling.
Further, in Process 1 via said SO3Introducing the smoke gas cooled by the evaporator into the fuming sulfuric acid SO3SO contained in flue gas absorbed by fuming sulfuric acid liquid in absorption tower3Gas, increasing the concentration of oleum, absorbed flue gas from the oleum SO3The top of the absorption tower is discharged to a sulfuric acid removal system for dry absorption process utilization.
Further, in the process 2, two second paths of circulating spiral plate type preheaters are arranged in series.
Further, in the process 2, SO volatilized from the high-concentration oleum in the oleum circulating tank3Gas is conveyed to SO through a pipeline3The gas absorber performs an absorption process.
Further, the SO in Process 23SO separation by evaporation in evaporator3Introducing the high-temperature acid solution after gas into the plate preheater to exchange heat with the acid solution in the plate preheater, and discharging the high-temperature acid solution after temperature reduction from the plate preheaterThe heat device enters the fuming sulfuric acid circulating tank.
Further, in the process 2, the area of the spiral plate type preheater and the medium are selected to be proper, the heat exchange is sufficient as much as possible, SO that the acid feeding and discharging in the second loop can perform sufficient heat exchange and save energy, and the SO is removed from the acid liquor after the temperature of the acid feeding is increased3The evaporator is favorable for evaporating and separating pure SO3The acid liquor with the lower acid temperature reduced returns to the fuming sulfuric acid circulating tank to indirectly reduce the first circulating temperature and remove the fuming sulfuric acid SO3The absorption tower is favorable for absorbing SO in the flue gas3。
Further, the temperature difference between the two media at the cold side after heat exchange of the spiral plate type preheater is less than 20 ℃.
Further, uncondensed SO from Process 33Gas enters the fuming sulfuric acid SO3And the acid return pipe of the absorption tower is contacted and absorbed with high-concentration fuming sulfuric acid in the acid return pipe, and then flows into the fuming sulfuric acid circulating groove together for recycling.
Further preferably, SO not condensed in Process 33Gas in oleum SO3The absorption tower acid return pipe is converged between 80 and 350mm below the elbow when entering the fuming sulfuric acid circulating tank, and is absorbed and dissolved by the high-concentration fuming sulfuric acid in the acid return pipe and then is sent to the fuming sulfuric acid circulating tank.
Further, the double-row micro-slope sprinkling-descending type condenser comprises a sprinkling-descending water pipe, a micro-slope pipeline and a water receiving tank which are sequentially arranged from top to bottom, wherein the micro-slope pipeline is formed by serially connecting two rows of straight pipes into a steel single pipeline which has the gradient of 1-3 degrees and continuously descends back and forth.
Further preferably, the distance between the upper and lower adjacent straight pipes on the micro-slope pipeline is 51-57 mm. And the upper end inlet of the micro-slope pipeline is connected with the SO3The top end and the lower end of the evaporator are respectively connected with the liquid SO3A finished product storage tank and the nicotinic acid absorption tower acid return pipe.
Preferably, the number of the sprinkling and precipitation pipes is two, a plurality of water outlet holes are uniformly distributed in the bottom of each sprinkling and precipitation pipe along the length direction of the sprinkling and precipitation pipe, the holes of the water outlet holes face downwards, the aperture is 5-15mm, and the distance between the water outlet holes and the top of the micro-slope pipeline is 20-40 mm.
Further preferably, the two sides of the micro-slope pipeline are respectively provided with an anti-splash water-retaining inclined fin plate, and the length direction of the anti-splash water-retaining inclined fin plate is consistent with the horizontal direction of the micro-slope pipeline.
Further preferably, the water in the water receiving tank flows into a water cooling tower of the sulfuric acid process system for circulation or is used as make-up water of the water cooling tower.
Further, process equipment SO3Evaporator, double-row micro-slope sprinkling type condenser and liquid SO3The horizontal heights of the finished product storage tank and the fuming sulfuric acid circulating tank are gradually reduced, and the SO is added3The liquid flows automatically between the process equipment.
The invention also provides a sulfuric acid system for producing liquid SO by using the process3The device comprises a fuming sulfuric acid circulating tank, a spiral plate type cooler and fuming sulfuric acid SO3Absorption tower, spiral plate type preheater and SO3Evaporimeter and double row slight slope drench and fall formula condenser, wherein:
the fuming sulfuric acid circulating tank is respectively connected with the spiral plate cooler and the spiral plate preheater through a circulating pump through pipelines so as to respectively convey the acid liquor to the spiral plate cooler for cooling treatment and to the spiral plate preheater for preheating treatment;
the spiral plate cooler is connected with the fuming sulfuric acid circulating tank through the absorption tower through a pipeline so as to contact and absorb the cooled acid liquid and the cooled flue gas into high-concentration fuming sulfuric acid, and the high-concentration fuming sulfuric acid flows back to the fuming sulfuric acid circulating tank through an acid return pipe;
the spiral plate type preheater is connected with the SO through a pipeline3The bottom of the evaporator is used for feeding the preheated acid liquid into the SO3Evaporating by an evaporator; the SO3The side part of the upper end socket of the evaporator is connected with the spiral plate type preheater through a pipeline so as to convey the fuming sulfuric acid liquid with the concentration reduced and flowing out after evaporation into the spiral plate type preheater to perform heat exchange with the acid feeding liquid of the spiral plate type heat exchanger; and
the SO3The top of the evaporator is connected with the double-row micro-slope sprinkling-falling type condenser through a pipeline SO as to evaporate the pure SO3Conveying the gas into the double-row micro-slope sprinkling-falling type condenser for condensation treatment, and condensing SO3The liquid flows into the liquid SO through the pipeline3A finished product storage tank; uncondensed SO3Gas enters the fuming sulfuric acid SO through a pipeline3And after the acid return pipe of the absorption tower is contacted and absorbed with high-concentration oleum in the acid return pipe, the oleum flows into the oleum circulating tank together for recycling.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
1) 2 spiral plate preheaters which are connected in series and have enough area and flow velocity are adopted to realize the full utilization of self heat and temperature rise, and the heated SO enters the shell3The evaporator is heated by the hot process flue gas of the sulfuric acid system and then heated, so that the boiling point of the nicotinic acid can be sufficiently reached for rapid evaporation, the heat of the hot process flue gas of the sulfuric acid system is fully utilized, the most convenient and energy-saving effect is realized, no extra energy consumption is realized, and the cost is lowest;
2) the adopted double-row micro-slope sprinkling type condenser is externally sprinkled with water and is not pressurized, and SO in the condenser is3Pressure, in case of leakage, SO3The water can not enter the condenser forever due to outward leakage, thus thoroughly avoiding the phenomenon that once the traditional shell and tube heat exchanger is leaked, the water enters SO3Violent reaction, heating and explosion accidents occur in the container storage tank and the pipeline, and the problems that the micro-seams of the traditional condenser tube array are immersed and corroded and are not easy to detect are solved; safe and can find the leakage point in time, once the double-row micro-slope sprinkling type condenser is exposed, because of SO3No matter the liquid or the gas is contacted with the air, white obvious smoke is generated immediately, and the treatment can be found quickly;
3) the double-row micro-slope sprinkling-falling type condenser can be completely cooled by water, namely, the water sprinkling-falling type condenser is extremely strong in effect compared with air cooling, and high in heat transfer coefficient, and the sprinkling-falling type condenser adopts the structure that the intermittent water-retaining fin plates are arranged on two sides, so that the water-moistening condition of the double-row pipes can be seen, the ventilation is not influenced, and water can be completely recovered while water splashing is prevented.
4) The double-row micro-slope sprinkling-falling type condenser with double rows of single-pipe runners and micro slopes which are closely arranged solves the problem of large volume of the condenser, the sprinkling is small, double rows of overflowing media can be the same in size through the single pipe, and the defects that the parallel connection of different flow rates is different and the condensation control is troublesome are avoided.
5) The outlet pipe of the double-row micro-slope sprinkling type condenser is connected with liquid SO3Finished product storage tank, fuming sulfuric acid SO also connected with nicotinic acid circulation tank3Acid return pipe of absorption tower, uncondensed SO3The gas can be flushed into the acid return pipe to be dissolved with the nicotinic acid in the pipe and reused, SO that the SO in the double-row micro-slope sprinkling-falling type condenser3The design accelerates the flow rate of the liquid, can completely liquefy only by increasing the water quantity, and has high capacity, high elasticity and high cooling efficiency;
6) in addition, even part of SO in the double-row micro-slope spraying-falling type condenser3Gas not being liquefied at all time, SO3The gas can be flushed into the acid return pipe for dissolution; the prior art only depends on the reduction of the condensation volume to the pushing speed, can not increase the water quantity to avoid freezing, has small operation elasticity and lower efficiency, and the invention is safe and reliable, breaks through the limitations and is a sulfuric acid system for producing liquid SO3The practical and safe process.
Drawings
FIG. 1 shows a process for producing liquid SO in a sulfuric acid system according to the present invention3The process flow schematic diagram of the practical and safe process;
FIG. 2 shows a process for producing liquid SO in a sulfuric acid system according to the present invention3The structural schematic diagram of the double-row micro-slope sprinkling-falling type condenser in the practical and safe process;
wherein the reference symbols are:
1-fuming sulfuric acid circulation tank; 2-a circulating pump; 3-a spiral plate cooler; 4-oleum SO3An absorption tower; 5-spiral plate type preheater; 6-SO3An evaporator; 7-double row micro-slope sprinkling type condenser, 71-sprinkling type water-dropping pipe, 72-micro-slope pipeline, 73-water receiving tank and 74-splash-proof water-retaining inclined fin plate; 8-liquid SO3And (5) a finished product storage tank.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example 1
Referring to FIG. 1, the present embodiment provides a sulfuric acid system for producing liquid SO3The practical and safe process specifically comprises the following steps:
in the process 1, hot flue gas generated by the sulfuric acid system process enters SO3In the evaporator 6, the SO3 is supplied with evaporation heat from the evaporator 6 via the SO3After heat exchange and temperature reduction of the evaporator 6, fuming sulfuric acid SO is introduced3In the absorption tower 4;
process 2 adopts circulating pump 2 to pump out the oleum in oleum circulation groove 1, divides two way circulations, and first way is carried to spiral plate cooler 3 and is cooled down the processing, and the second way is carried to spiral plate preheater 5 and is carried out the intensification processing, specifically:
the first path of fuming acid liquid cooled by the spiral plate cooler 3 is conveyed to fuming sulfuric acid SO3An absorption tower 4 for absorbing the introduced fuming sulfuric acid SO3SO contained in flue gas in the absorption tower 43Returning the obtained high-concentration oleum to the oleum circulating tank 1 by the gas to supplement SO of the oleum circulating tank 1 with oleum3Content (c);
the second path of fuming acid liquor preheated and heated by the spiral plate type preheater 5 is conveyed to SO3The evaporator 6 is used for evaporating and separating out pure SO3The gas and the high-temperature fuming sulfuric acid liquid with reduced concentration after evaporation flow out through the spiral plate type preheater 5 and return to the fuming sulfuric acid circulating tank 1;
process 3, SO3The evaporator 6 is heated to evaporate pure SO separated from fuming sulfuric acid3The gas is introduced into a double-row micro-slope sprinkling-falling type condenser 7 for cooling treatment, and all or most of SO3The gas is condensed into SO3Liquid, flowing into liquid SO3The finished product is obtained in the finished product storage tank 8 without condensed SO3The gas enters fuming sulfuric acid SO3Dissolving in acid return pipe of absorption towerAdding into oleum for reuse.
As a technical solution of this embodiment, as shown in FIG. 1, the SO in the process 13The flue gas cooled by the evaporator 6 is introduced into the fuming sulfuric acid SO3SO contained in flue gas absorbed by fuming sulfuric acid liquid in the absorption tower 43Gas, increasing the concentration of oleum, absorbed flue gas from the oleum SO3The top of the absorption tower 4 is discharged to a sulfuric acid removal system for dry absorption process utilization.
Furthermore, the SO3SO evaporated by the evaporator 63The acid foam is removed by the cyclone demister on the top of the cyclone demister, the acid foam is recycled, and the ratio of the pipe diameter of an outlet of the cyclone demister to the cylinder diameter of the cyclone demister is 2/7-1/3.
As a technical solution of this embodiment, the SO in the process 23SO is evaporated and separated in the evaporator 63And introducing the high-temperature acid liquid after gas into the spiral plate type preheater 5, exchanging heat with the low-temperature acid liquid in the spiral plate type preheater 5, and cooling the high-temperature acid liquid out of the plate type preheater 5 and then entering the fuming sulfuric acid circulating tank 1.
As a solution of this embodiment, as shown in fig. 1, the spiral plate preheater on the second circulation loop must have sufficient efficiency and area, and in the process 2, two spiral plate preheaters 5 are arranged in series. The two spiral plate type preheaters 5 which are arranged in series have better heat exchange effect, and can fully utilize the heat of the preheaters, reduce the temperature of the sulfuric acid circulation tank 1 for returning smoke and improve the SO of the smoke-removing sulfuric acid3The temperature of the evaporator 6 is fully raised and then enters SO3The evaporator 6 is heated by the hot flue gas of the sulfuric acid system process and then heated, SO that the boiling point of fuming sulfuric acid can be sufficiently reached and pure SO can be quickly evaporated3The gas, the best use of self heat exchange of fuming sulfuric acid circulation and the use of the heat of hot flue gas of the sulfuric acid system process are the most convenient and energy-saving, and the cost is the lowest.
As a technical scheme of the embodiment, in the process 2, a small amount of SO volatilized from high-concentration oleum in the oleum circulation tank 13Gas is pumped by using the negative pressure of a sulfuric acid production system and is conveyed to SO through a pipeline3The gas absorber carries out absorption treatment to prevent the fuming sulfuric acid from smoking outside the circulating tank.
As a technical scheme of the embodiment, in the process 3, the uncondensed SO passes through the double-row micro-slope sprinkling type condenser 73Gas enters the fuming sulfuric acid SO3In the acid return pipe of the absorption tower 4, the acid return pipe is contacted with high-concentration oleum in the acid return pipe for absorption, and then the acid return pipe and the high-concentration oleum flow into the oleum circulation tank 1 for cyclic utilization.
As a technical solution of this embodiment, in the process 2, the area and the medium flow rate of the spiral plate preheater 5 are sufficient, so that sufficient heat exchange can be realized, and the temperature difference between the two media on the cold side after heat exchange by the spiral plate preheater 5 is less than 20 ℃.
As a technical proposal of the embodiment, in the process 3, SO which is not condensed3Gas in oleum SO3The return acid pipe of the absorption tower 4 is converged between 80 mm and 350mm below the elbow when entering the fuming sulfuric acid circulating tank 1, and is absorbed and dissolved by the high-concentration fuming sulfuric acid in the return acid pipe and then is sent to the fuming sulfuric acid circulating tank 1.
As a preferred technical solution of this embodiment, as shown in fig. 2, the double-row micro-slope shower-falling type condenser includes a shower-falling water pipe 71, a micro-slope pipeline 72 and a water receiving tank 73, which are sequentially arranged from top to bottom, wherein the micro-slope pipeline 72 is formed by two rows of steel single pipelines which are serially connected to form a continuous back-and-forth falling pipeline with a slope of 1 to 3 °, and the area corresponds to the capacity. Preferably, the gradient of the steel single pipeline is 1.5-2.5 degrees, and the upper end inlet of the micro-slope pipeline 72 is connected with the SO3The top end of the upper end socket of the evaporator 6 and the outlet at the lower end are respectively connected with the liquid SO3Finished product storage tank 8 and oleum SO3On the acid return pipe of the absorption tower 4.
As a preferable technical scheme of the embodiment, as shown in FIG. 2, the distance between the upper and lower adjacent straight pipes on the micro-slope pipeline 72 is 51-57 mm. Preferably, the distance between the adjacent upper and lower pipelines is 51mm, SO3The evaporator is shown in the figure 2, the pipe spacing is large, the actual pipe spacing is small for indicating the structure, and less water splashed outside when the shower water falls on each pipe is tightly promoted; the design of single pipeline can make double rowsThe size of the overflowing medium is the same, so that the defects of different flow rates of the parallel pipes and troublesome condensation control are avoided.
As another preferable technical solution of this embodiment, the drenching precipitation liquid recovered in the water receiving tank 73 automatically flows into the cooling tower circulation tank or is used as water supplement of the cooling tower circulation tank.
Adopts a double-row micro-slope sprinkling type condenser, water is sprinkled outside, no pressure is generated, and SO in the condenser is generated3Pressure, in case of leakage, SO3The water can not enter the condenser forever due to outward leakage, thus thoroughly avoiding the phenomenon that once the traditional shell and tube heat exchanger is leaked, the water enters SO3The violent reaction, heating and explosion accidents occur in the container storage tank and the pipeline, the problem that the micro-slits of the traditional condenser tube nest are immersed and corroded and are not easy to be noticed is avoided, the leakage point can be safely and timely found, once the double-row micro-slope sprinkling type condenser is exposed, the SO is used for preventing the leakage of the condensed water3Treatment was soon discovered, whether liquid or gas was in contact with air, producing a visibly white smoke.
In addition, two sides of the double-row micro-slope sprinkling condenser 7 are provided with splash-proof water-retaining inclined fin plates 74 which are distributed at intervals up and down, the splash-proof water-retaining inclined fin plates 74 are horizontally arranged, and the splash-proof water-retaining inclined fin plates 74 are inclined and opened outwards. The water wetting condition of the micro-slope pipeline 72 can be seen through the interval between the upper splash-proof water retaining inclined fin plates 74 and the lower splash-proof water retaining inclined fin plates 74, ventilation is not affected, water can be completely recycled while water splashing is prevented, the double-row micro-slope sprinkling-falling condenser can be completely cooled by water, namely, water sprinkling-falling cooling is greatly stronger than air cooling effect, heat transfer coefficient is high, the sprinkling condition can be directly observed, and inspection is convenient.
As a technical solution of this embodiment, there are two of the sprinkling and precipitation pipes 71, the bottom of each of the sprinkling and precipitation pipes 71 is provided with a plurality of uniformly distributed water outlet holes along the length direction thereof, the holes of the water outlet holes are downward, the aperture is 5-15mm, and the distance between the water outlet holes and the top of the micro-slope pipe 72 is 20-40 mm; preferably, the aperture of the water outlet hole is 8-12mm, the distance between the water outlet hole and the top of the micro-slope pipeline 72 is 25-32mm, the size of the water can be seen, all the holes can uniformly discharge water simultaneously, the size of the water regulating valve is arranged on the sprinkling and descending water pipe 71, and partial water discharge can be controlled according to needs.
In this example, the SO is described in the Process flow Equipment3Evaporator 6, double-row micro-slope sprinkling type condenser 7 and liquid SO3The finished product storage tank 8 and the fuming sulfuric acid circulating tank 1 are gradually reduced in level, and the SO is3The liquid realizes self-flow among all process flow devices.
Production of liquid SO of this example3The practical and safe process fully and efficiently realizes the utilization and cyclic utilization of system heat, and the anhydrous dry hot flue gas of the sulfuric acid system is utilized to safely heat SO3The evaporator and the circulating fuming sulfuric acid liquid carry out self sufficient heat exchange through improving the heat exchange capacity of the preheater, and particularly, a single-tube double-row sprinkling and descending type condenser is created for condensation, so that the production cost is greatly reduced, the reliability and the safety are improved, and the problems of insufficient evaporation heat and the safety and the high efficiency of the condenser are effectively solved.
Example 2
Based on the above example 1, this example provides a sulfuric acid system for producing liquid SO according to the above process3As shown in fig. 1 and 2, the device mainly comprises a fuming sulfuric acid circulating tank 1, a spiral plate cooler 3 and fuming sulfuric acid SO3Absorption tower 4, spiral plate type preheater 5 and SO3An evaporator 6 and a double-row micro-slope sprinkling type condenser 7.
In this embodiment, the fuming sulfuric acid circulation tank 1 is connected with the spiral plate cooler 3 and the spiral plate preheater 5 through the circulating pump 2 via the pipeline, so as to respectively convey the acid liquid in the fuming sulfuric acid circulation tank to the spiral plate cooler 3 for cooling and to the spiral plate preheater 5 for preheating; the spiral plate cooler 3 passes through the fuming sulfuric acid SO through a pipeline3The absorption tower 4 is connected with the fuming sulfuric acid circulating tank 1 so as to contact and absorb the cooled acid liquid and the flue gas into high-concentration fuming sulfuric acid, and the high-concentration fuming sulfuric acid flows back to the fuming sulfuric acid circulating tank 1 through an acid return pipe;
in this embodiment, the plate preheater 5 is connected to the SO through a pipe3The bottom of the evaporator 6 to feed the preheated acid liquid into the SO3The evaporator 6 carries out evaporation treatment; the SO3Evaporation ofThe side part of the upper end socket of the device 6 is connected with the spiral plate type preheater 5 through a pipeline so as to convey the fuming sulfuric acid solution with the concentration reduced and flowed out after evaporation into the spiral plate type preheater 5 to perform heat exchange with the concentrated acid solution to be evaporated. The SO3The top of the upper end socket of the evaporator 6 is connected with the double-row micro-slope spraying-falling type condenser 7 through a pipeline SO as to evaporate the pure SO3Conveying the gas into the double-row micro-slope sprinkling-falling type condenser 7 for condensation treatment, and condensing SO3The liquid flows into the liquid SO through the pipeline3A finished product storage tank 8; uncondensed SO3Gas enters the fuming sulfuric acid SO through a pipeline3And after the acid return pipe of the absorption tower 4 is contacted and absorbed with high-concentration oleum in the acid return pipe, the oleum flows into the oleum circulating tank 1 together for recycling.
In this embodiment, as shown in fig. 2, as in embodiment 1, the double-row micro-slope spray-drop condenser 7 includes a spray-drop water pipe 71, a micro-slope pipeline 72 and a water receiving tank 73, which are sequentially arranged from top to bottom, wherein the micro-slope pipeline 72 is composed of two rows of steel single pipelines which are serially connected to form a continuous back-and-forth descending slope with a slope of 1-3 °, and the area corresponds to the capacity. Preferably, the gradient of the steel single pipeline is 1.5-2.5 degrees, and the upper end inlet of the micro-slope pipeline 72 is connected with the SO3The top end of the upper end socket of the evaporator 6 and the outlet at the lower end are respectively connected with the liquid SO3Finished product storage tank 8 and oleum SO3On the acid return pipe of the absorption tower 4.
In the present embodiment, as shown in fig. 2, the distance between the upper and lower adjacent straight pipes on the micro-slope pipeline 72 is 51-57 mm. Preferably, the distance between the adjacent upper and lower pipelines is 51mm, SO3The schematic diagram of the evaporator shown in the figure 2 has larger spacing, is used for illustrating the structure, has small actual spacing, and achieves the purposes of tight and compact structure and less splashing water when the shower water falls onto each pipe; the single-pipeline design can make the double-row medium size of overflowing the same, avoid parallelly connected each pipe flow volume to differ, the trouble disadvantage of condensation control. The water from the water receiving tank 73 flows into a water cooling tower of a sulfuric acid process system for circulation or is used as make-up water of the water cooling tower.
In this embodiment, a double-row micro-slope spray-falling type condenser is adopted, water is sprayed outside, no pressure is applied, and SO in the condenser is3Pressure, in case of leakage, SO3The water can not enter the condenser forever due to outward leakage, thus thoroughly avoiding the phenomenon that once the traditional shell and tube heat exchanger is leaked, the water enters SO3The violent reaction, heating and explosion accidents occur in the container storage tank and the pipeline, the problem that the micro-slits of the traditional condenser tube nest are immersed and corroded and are not easy to be noticed is avoided, the leakage point can be safely and timely found, once the double-row micro-slope sprinkling type condenser is exposed, the SO is used for preventing the leakage of the condensed water3Treatment was soon discovered, whether liquid or gas was in contact with air, producing a visibly white smoke.
In addition, the two sides of the double-row micro-slope sprinkling condenser 7 are provided with intermittent splash-proof water-retaining inclined fin plates 74, and the length direction of the splash-proof water-retaining inclined fin plates 74 is consistent with the horizontal direction of the slope direction of the micro-slope pipeline 72. The double-row pipe water moistening condition can be seen through the interval between the upper splash-proof water retaining inclined fin plates 74 and the lower splash-proof water retaining inclined fin plates 74, ventilation is not affected, water can be completely recycled while water splashing is prevented, the double-row micro-slope sprinkling type condenser 7 can be completely cooled by water, safety is not worried about leakage at all, namely, water sprinkling cooling is achieved, the effect is stronger than that of air cooling, the heat transfer coefficient is high, the sprinkling condition can be directly observed, and the inspection is convenient.
As a technical solution of this embodiment, there are two of the sprinkling and precipitation pipes 71, the bottom of each of the sprinkling and precipitation pipes 71 is provided with a plurality of uniformly distributed water outlet holes along the length direction thereof, the holes of the water outlet holes are downward, the aperture is 5-15mm, and the distance between the water outlet holes and the top of the micro-slope pipe 72 is 20-40 mm; preferably, the aperture of the water outlet hole is 8-12mm, the distance between the water outlet hole and the top of the micro-slope pipeline 72 is 25-32mm, the size of the water can be seen, all the holes can uniformly discharge water simultaneously, the size of the water regulating valve is arranged on the sprinkling and descending water pipe 71, and partial water discharge can be controlled according to needs.
In this example, the SO is described in the Process flow Equipment3A double-row micro-slope sprinkling type condenser 7 at the top of the evaporator 6 and liquid SO3The finished product storage tank 8 and the fuming sulfuric acid circulating tank 1 are gradually reduced in level, and the SO is3The liquid realizes self-flow among all process flow devices.
In the embodiment, fuming sulfuric acid is beaten out by the circulating pump to be divided into two paths of circulation, iAfter the passage is cooled by the spiral plate cooler, the fuming sulfuric acid SO is removed3The absorption tower absorbs SO in the flue gas3The concentration of fuming sulfuric acid is improved; after the temperature of the liquid is raised through a spiral plate type preheater, the liquid goes to the evaporator to evaporate pure SO3Gas, pure SO3The gas is removed from the double-row micro-slope sprinkling type condenser to be condensed safely and efficiently to prepare SO3Liquid, and the evaporator evaporates pure SO3The hot fuming sulfuric acid solution with reduced gas concentration flows out of SO3After the evaporator, the gas flows back to the fuming sulfuric acid circulation tank for cyclic utilization after the full heat exchange of the two-stage spiral preheater, the system heat cyclic utilization is realized fully and efficiently, the production cost is greatly reduced, and the problems of safety, high efficiency and insufficient evaporation heat of the condenser are effectively solved.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (10)
1. Sulfuric acid system production liquid SO3The practical and safe process is characterized by comprising the following processes;
in the process 1, dry hot flue gas generated by the sulfuric acid system process passes through SO3In the evaporator (6) is SO3The evaporator (6) provides evaporation heat;
2, fully preheating and heating the fuming sulfuric acid solution by a spiral plate type preheater (5), and conveying the fuming sulfuric acid solution to SO3The evaporator (6) is heated for SO3Evaporating, and discharging SO from high-temperature fuming sulfuric acid solution with reduced concentration after evaporation3The evaporator (6) returns to pass through the spiral plate type preheater (5), fully preheats concentrated fuming sulfuric acid to be evaporated, and flows back to the fuming sulfuric acid circulating tank (1) after being cooled;
process 3, SO3The evaporator (6) is heated to evaporate fuming sulfuric acid to separate out pure SO3Gas is introduced into the double-row micro-slope showerThe condenser (7) is used for condensing all or most of SO3The gas is condensed into SO3Liquid, flowing into liquid SO3The finished product is obtained in a finished product storage tank (8) without condensed SO3The gas enters fuming sulfuric acid SO3The acid return pipe of the absorption tower (4).
2. Sulfuric acid system production liquid SO according to claim 13The practical and safe process is characterized in that in the process 2, two spiral plate type preheaters (5) are arranged in series.
3. Sulfuric acid system production liquid SO according to claim 13The practical and safe process is characterized in that in the process 2, the temperature difference between the two media at the cold side is less than 20 ℃ after the heat exchange of the spiral plate type preheater (5).
4. Sulfuric acid system production liquid SO according to claim 13Is characterized in that in the process 3, SO which is not condensed is3Gas in oleum SO3The return acid pipe of the absorption tower is converged between 80 and 350mm below the elbow when entering the fuming sulfuric acid circulating tank (1), and is absorbed and dissolved by high-concentration fuming sulfuric acid in the return acid pipe and then is sent into the fuming sulfuric acid circulating tank (1).
5. Sulfuric acid system production liquid SO according to claim 13The practical and safe process is characterized in that the double-row micro-slope sprinkling-falling type condenser (7) comprises a sprinkling-falling water pipe (71), a micro-slope pipeline (72) and a water receiving tank (73) which are sequentially arranged from top to bottom, wherein the micro-slope pipeline (72) is formed by connecting two rows of straight pipes in series to form a steel single pipeline which has a slope of 1-3 degrees and continuously descends back and forth.
6. Sulfuric acid system production liquid SO according to claim 53The practical and safe process is characterized in that the distance between the upper and lower adjacent straight pipes on the micro-slope pipeline (72) is 51-57 mm.
7. Sulfuric acid system production liquid SO according to claim 53The practical and safe process is characterized in that the number of the sprinkling and precipitation pipes (71) is two, a plurality of uniformly distributed water outlet holes are formed in the bottom of each sprinkling and precipitation pipe (71) along the length direction of the sprinkling and precipitation pipe, the holes of the water outlet holes face downwards, the hole diameter is 5-15mm, and the distance between the holes and the top of the micro-slope pipeline (72) is 20-40 mm.
8. Sulfuric acid system production liquid SO according to claim 53The practical and safe process is characterized in that splash-proof water-retaining oblique fin plates (74) are respectively arranged on two sides of the micro-slope pipeline (72), and the length direction of the splash-proof water-retaining oblique fin plates (74) is consistent with the level of the direction of the micro-slope pipeline (72).
9. Sulfuric acid system production liquid SO according to claim 53The practical and safe process is characterized in that the water in the water receiving tank (73) flows into a water cooling tower of a sulfuric acid process system for circulation or is used as make-up water of the water cooling tower.
10. Sulfuric acid system production liquid SO according to claim 13The practical and safe process is characterized in that in the process 3, process flow equipment SO3An evaporator (6), a double-row micro-slope sprinkling type condenser (7) and liquid SO3The horizontal heights of the finished product storage tank (8) and the fuming sulfuric acid circulating tank (1) are gradually reduced, and the SO3The liquid flows automatically between the process equipment.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2863760Y (en) * | 2005-09-27 | 2007-01-31 | 上海宁松热能环境工程有限公司 | Apparatus for preparation liquid sulfur trioxide from oleum |
| CN101381075A (en) * | 2008-10-15 | 2009-03-11 | 湖北鑫慧化工有限公司 | Liquid sulfur trioxide and method for producing high concentration fuming sulfuric acid |
| CN101759157A (en) * | 2010-01-08 | 2010-06-30 | 山东聊城鲁西化工第六化肥有限公司 | Process and equipment using SO3 furnace gas as heating carrier for evaporating SO3 |
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2019
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2863760Y (en) * | 2005-09-27 | 2007-01-31 | 上海宁松热能环境工程有限公司 | Apparatus for preparation liquid sulfur trioxide from oleum |
| CN101381075A (en) * | 2008-10-15 | 2009-03-11 | 湖北鑫慧化工有限公司 | Liquid sulfur trioxide and method for producing high concentration fuming sulfuric acid |
| CN101759157A (en) * | 2010-01-08 | 2010-06-30 | 山东聊城鲁西化工第六化肥有限公司 | Process and equipment using SO3 furnace gas as heating carrier for evaporating SO3 |
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