CN110589779B - Sulfuric acid system production liquid SO 3 Practical and safe process of (2) - Google Patents
Sulfuric acid system production liquid SO 3 Practical and safe process of (2) Download PDFInfo
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- CN110589779B CN110589779B CN201911060661.2A CN201911060661A CN110589779B CN 110589779 B CN110589779 B CN 110589779B CN 201911060661 A CN201911060661 A CN 201911060661A CN 110589779 B CN110589779 B CN 110589779B
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- 239000007788 liquid Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims description 73
- 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 118
- 239000007789 gas Substances 0.000 claims abstract description 47
- 238000001816 cooling Methods 0.000 claims abstract description 24
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 22
- 239000003546 flue gas Substances 0.000 claims abstract description 22
- 238000003860 storage Methods 0.000 claims abstract description 18
- 230000008020 evaporation Effects 0.000 claims abstract description 14
- 230000005494 condensation Effects 0.000 claims abstract description 12
- 238000009833 condensation Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 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 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 74
- 239000002253 acid Substances 0.000 claims description 51
- 238000010521 absorption reaction Methods 0.000 claims description 37
- 230000026676 system process Effects 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 125000004122 cyclic group Chemical group 0.000 abstract description 2
- 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
- 238000004064 recycling Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000006260 foam Substances 0.000 description 6
- 239000000779 smoke Substances 0.000 description 5
- 238000010586 diagram Methods 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
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000004880 explosion 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
- 230000001276 controlling effect Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000009736 wetting Methods 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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000010025 steaming Methods 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
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000001502 supplementing effect Effects 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 sulfuric acidSystem for producing liquid SO 3 The practical and safe process of (2) comprises the following steps: process 1, passing dry and hot flue gas over SO 3 In the evaporator, is SO 3 The evaporator provides the heating value; step 2, the fuming sulfuric acid liquid after being fully preheated and heated by the spiral plate type preheater is conveyed to SO 3 The evaporator is heated to carry out SO 3 Evaporating, enabling the evaporated high-temperature fuming sulfuric acid liquid with reduced concentration to pass through a spiral plate type preheater, fully preheating the fuming sulfuric acid to be evaporated, cooling and then flowing back to a fuming sulfuric acid circulation tank; process 3, SO 3 The evaporator is heated to evaporate fuming sulfuric acid to separate out pure SO 3 The gas is introduced into a double-row micro-slope shower-drop condenser for condensation treatment and is condensed into SO 3 Liquid, self-flowing into liquid SO 3 And obtaining a product from the finished product storage tank. The invention produces liquid SO 3 The practical safety process of the utility model realizes the utilization and cyclic utilization of the heat of the system with full high efficiency, greatly reduces the production cost, improves the reliability and safety, and effectively solves the problems of insufficient evaporation heat and the safety and high efficiency of the condenser.
Description
Technical Field
The invention relates to the technical field of sulfuric acid production, in particular to a sulfuric acid system for producing liquid SO 3 Is practical and safe.
Background
Liquid SO 3 The method is mainly used as a sulfonating agent and is an intermediate product for preparing high-concentration fuming sulfuric acid and chlorosulfonic acid. Currently, a large amount of sulfur trioxide in China is used for manufacturing sodium alkylbenzenesulfonate and sulfonated lubricating oilMaking white oil and biopharmaceutical. The fuming sulfuric acid with high concentration is mainly used as sulfonating agent for sulfonation reaction, smoke bomb and the like. SO (SO) 3 The liquid has strong volatility, is easy to freeze, can not meet water, belongs to dangerous chemicals, and therefore, the production safety is important.
Three main problems exist in the existing production method: firstly, the heat required by evaporation is often insufficient, the evaporation and the yield are affected, and some of the heat has to be heated by adopting steam of about 0.8MPa, so that the energy consumption also brings risks; secondly, the condensation capacity is small and limited, the cooling water is large or cold, the solidification and blockage faults are easy to occur, and the treatment is very troublesome; the cooling water is small or the heat output is affected, SO 3 The gas is influenced by the condensing speed, so that the quantity entering the condenser is limited, the gas cannot directly pass through the condenser, and the gas must be condensed; thirdly, the biggest problem is that the high-efficiency cooling and the safety of the condenser are taken into consideration, no good method is provided, namely, the high water cooling effect is required, the water leakage is afraid of accidents caused, the air cooling is adopted for safety, the efficiency is extremely low, and the air cooling is particularly obvious in summer.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a sulfuric acid system for producing liquid SO 3 Is practical and safe.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a sulfuric acid system for producing liquid SO 3 The practical and safe process of (2) comprises the following steps:
in the process 1, dry hot flue gas generated by a sulfuric acid system process is subjected to SO 3 In the evaporator, is SO 3 The evaporator provides the heating value;
step 2, the fuming sulfuric acid liquid after being fully preheated and heated by the spiral plate type preheater is conveyed to SO 3 The evaporator is heated to carry out SO 3 Evaporating, and flowing out SO from the high-temperature fuming sulfuric acid liquid with reduced concentration after evaporation 3 The evaporator returns to pass through a spiral plate type preheater to fully preheat the fuming sulfuric acid to be evaporated, and the fuming sulfuric acid returns to a fuming sulfuric acid circulation tank after being cooled;
process 3, SO 3 The evaporator is heated to evaporate fuming sulfuric acid to separate out pure SO 3 Introducing the gas into a double-row micro-slope shower-drop condenser for condensation treatment, and completely or mostly treating SO 3 The gas is condensed to SO 3 Liquid, self-flowing into liquid SO 3 The finished product storage tank obtains the product without condensed SO 3 The gas enters fuming sulfuric acid SO 3 The acid return pipe of the absorption tower.
Further, the sulfuric acid system produces liquid SO 3 The practical and safe process of (3) comprises the following steps:
in the process 1, hot flue gas generated by a sulfuric acid system process is subjected to SO 3 In the evaporator, is the SO 3 An evaporator for providing a heating value of the steam, the SO 3 The flue gas after heat exchange and temperature reduction of the evaporator is introduced into fuming sulfuric acid SO 3 An absorption tower;
step 2, a circulating pump is adopted to pump out fuming sulfuric acid liquid in a fuming sulfuric acid circulating tank into two paths of circulation, the first path of circulation is conveyed to a spiral plate type cooler for cooling treatment, and the other path of circulation is conveyed to a spiral plate type preheater for heating treatment; specifically:
the first path of fuming sulfuric acid liquid cooled by the spiral plate type cooler is conveyed to fuming sulfuric acid SO 3 An absorption tower for absorbing the SO of the fuming sulfuric acid 3 SO contained in flue gas in absorption tower 3 The gas, the high concentration fuming sulfuric acid obtained returns to the fuming sulfuric acid circulation tank, and the fuming sulfuric acid circulation tank is supplemented with SO of fuming sulfuric acid liquid 3 The content is as follows;
the second path of fuming acid liquid preheated by the spiral plate type preheater is conveyed to SO 3 Evaporating and separating out pure SO by an evaporator 3 High temperature fuming sulfuric acid liquid with reduced concentration after evaporation of gas flowing out of SO 3 The evaporator returns to the fuming sulfuric acid circulation tank through the spiral plate type preheater;
process 3: SO (SO) 3 Evaporating fuming sulfuric acid by an evaporator to separate out pure SO 3 Introducing the gas into a double-row micro-slope shower-drop condenser for cooling treatment, and completely or mostly treating SO 3 The gas is condensed to SO 3 Liquid, self-flowing into liquid SO 3 Obtaining a product from a finished product storage tank; SO without condensation 3 The gas enters fuming sulfuric acidSO 3 And the acid return pipe of the absorption tower is dissolved into fuming sulfuric acid solution to enter a fuming sulfuric acid circulation tank for recycling.
Further, in process 1 via the SO 3 Introducing the smoke cooled by the evaporator into the fuming sulfuric acid SO 3 SO contained in flue gas is absorbed by fuming sulfuric acid liquid in absorption tower 3 Gas, increasing the concentration of fuming sulfuric acid, and absorbing the flue gas from the fuming sulfuric acid SO 3 And the dry absorption procedure of the sulfuric acid system discharged from the top of the absorption tower is utilized.
Further, in the process 2, the second circulating screw plate type preheater is two and is arranged in series.
Further, SO volatilized by high-concentration oleum in the oleum circulation tank in the process 2 3 The gas being transported to SO by a pipeline 3 The gas absorber performs an absorption process.
Further, the SO in Process 2 3 Evaporating and separating SO in evaporator 3 And introducing the high-temperature acid liquor after gas into the plate-type preheater, exchanging heat with the acid liquor in the plate-type preheater, and cooling the high-temperature acid liquor and then discharging the high-temperature acid liquor out of the plate-type preheater to enter the fuming sulfuric acid circulation tank.
Further, in the process 2, the proper spiral plate type preheater area and medium flow speed are selected, heat exchange is as full as possible, SO that the upper acid and the lower acid in the second loop can be fully exchanged, energy is saved, and the SO is removed from the acid liquor after the acid temperature is increased 3 The evaporator is favorable for evaporating and separating out pure SO 3 The acid liquor with the lowered acid temperature returns to the fuming sulfuric acid circulation tank, the first path of circulation temperature is indirectly lowered, and fuming sulfuric acid SO is removed 3 An absorption tower is favorable for absorbing SO in the flue gas 3 。
Further, the temperature difference between the two media at the cold side after heat exchange by the spiral plate type preheater is less than 20 ℃.
Further, SO that is not condensed in Process 3 3 Gas enters the fuming sulfuric acid SO 3 And after contacting and absorbing the fuming sulfuric acid with high concentration in the acid return pipe, the fuming sulfuric acid flows into the fuming sulfuric acid circulation tank together for recycling.
Further preferably, the SO that is not condensed in Process 3 3 Gas in fuming sulfuric acid SO 3 The acid return pipe of the absorption tower is converged between 80 mm and 350mm below an elbow when entering the fuming sulfuric acid circulation tank, absorbed and dissolved by high-concentration fuming sulfuric acid in the acid return pipe, and then sent into the fuming sulfuric acid circulation tank.
Further, the double-row micro-slope shower-drop condenser comprises a shower-drop 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 connecting two rows of straight pipes in series to form a steel single pipeline with the gradient of 1-3 degrees and continuously descending back and forth.
Further preferably, the distance between the upper straight pipe and the lower straight pipe on the micro-slope pipeline is 51-57mm. And the upper end inlet of the micro-slope pipeline is connected with the SO 3 The outlets at the top end and the lower end of the evaporator are respectively connected with the liquid SO 3 And the finished product storage tank and the nicotinic acid absorption tower acid return pipe.
Further preferably, the number of the shower and drop pipes is two, the bottom of each shower and drop pipe is provided with a plurality of evenly distributed water outlet holes along the length direction of the shower and drop pipe, 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 pipeline is 20-40mm.
Further preferably, splash-proof water-retaining inclined wing plates are respectively arranged on two sides of the micro-slope pipeline, and the length direction of the splash-proof water-retaining inclined wing plates is consistent with the horizontal direction of the micro-slope pipeline.
It is further preferred that the water in the water receiving tank flows into a cooling tower of a sulfuric acid process system for circulation or is used as make-up water for the cooling tower.
Further, process flow equipment SO 3 Evaporator, double-row micro-slope shower-drop condenser and liquid SO 3 The level of the finished product storage tank and the fuming sulfuric acid circulation tank is gradually reduced, and the SO 3 The liquid realizes self-flow between the process flow equipment.
The invention also provides a sulfuric acid system for producing liquid SO by the process 3 Comprises a fuming sulfuric acid circulating tank, a spiral plate type cooler and fuming sulfuric acid SO 3 Absorption tower, spiral plate type preheater and SO 3 Evaporator and double little slope drenches and falls formula condenser, wherein:
the fuming sulfuric acid circulation tank is connected with the spiral plate cooler and the spiral plate preheater through pipelines through circulation pumps respectively so as to convey acid liquor to the spiral plate cooler for cooling treatment and the spiral plate preheater for preheating treatment respectively;
the spiral plate type cooler is connected with the fuming sulfuric acid circulation tank through a pipeline by the absorption tower so as to absorb cooled acid liquor and cooled flue gas into high-concentration fuming sulfuric acid in a contact way, and the high-concentration fuming sulfuric acid flows back to the fuming sulfuric acid circulation tank through an acid return pipe;
the spiral plate type preheater is connected with the SO through a pipeline 3 The bottom of the evaporator is used for feeding the preheated acid liquor into the SO 3 The evaporator performs evaporation treatment; the SO 3 The 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 fuming sulfuric acid liquid with reduced concentration after evaporation to the spiral plate type preheater to exchange heat with the upper acid liquid of the spiral plate type heat exchanger; and
the SO 3 The top of the evaporator is connected with the double-row micro-slope shower-drop condenser through a pipeline SO as to evaporate pure SO 3 The gas is conveyed into the double-row micro-slope shower-drop condenser for condensation treatment, and condensed SO 3 Liquid flow into liquid SO through pipeline 3 A finished product storage tank; uncondensed SO 3 Gas enters the fuming sulfuric acid SO through a pipeline 3 The acid return pipe of the absorption tower is contacted with the fuming sulfuric acid with high concentration in the acid return pipe for absorption, and then flows into the fuming sulfuric acid circulation tank together for recycling.
Compared with the prior art, the invention has the following technical effects:
1) The spiral plate type preheater with enough area and flow speed and 2 series connection can realize the full utilization of self heat to raise the temperature, and the heat enters SO after the temperature is raised 3 The evaporator can heat and raise the temperature by the process hot flue gas of the sulfuric acid system, so that the boiling point of the nicotinic acid can be sufficiently reached to evaporate rapidly,the full utilization of the heat of the hot flue gas of the sulfuric acid system process is the most convenient and energy-saving, has no extra energy consumption and has the lowest cost;
2) Double-row micro-slope shower-drop type condenser, outer shower water, no pressure and SO in the condenser 3 Pressurized, SO upon leakage 3 The water leaks outwards, the water can not enter the condenser forever, once the traditional tube-in-tube heat exchanger leaks, the water can not enter SO 3 The severe reaction heating explosion accident occurs in the container storage tank and the pipeline, and the problems that the traditional condenser tube array micro-seam is immersed and corroded and is not easy to be perceived are avoided; the leakage point can be found safely and timely, and once the double-row micro-slope shower-drop condenser is exposed, the SO is generated 3 The contact of the liquid or the gas with the air can generate white obvious smog immediately, and the treatment can be discovered quickly;
3) The double-row micro-slope spray-descending condenser can be completely cooled by water, namely, the water spray-descending temperature is extremely higher than the air cooling effect, the heat transfer coefficient is high, the spray-descending condenser adopts the intermittent water retaining fin plates at two sides, the double-row pipe water wetting condition can be seen, ventilation is not influenced, and water can be fully recycled while water is splashed.
4) The double-row micro-slope showering-descending condenser with the single-tube flow channels which are closely arranged and provided with micro-slopes solves the problem that the condenser is large in size, showering water is splashed out little, the double-row overflowing medium can be the same in size by the single tube, and the defects of different parallel connection discharge amounts and troublesome condensation control are avoided.
5) The outlet pipe of the double-row micro-slope shower-drop condenser is connected with liquid SO 3 A finished product storage tank is also connected with fuming sulfuric acid SO of the nicotinic acid circulation tank 3 Acid return pipe of absorption tower, uncondensed SO 3 The gas can be flushed into the acid return pipe to be dissolved and reused with nicotinic acid in the pipe, thus leading the SO in the double-row micro-slope shower-drop condenser to be realized 3 The overflow is accelerated, the heat transfer coefficient is high, the condensed liquid is pushed away by the uncondensed gas, the design accelerates the flow rate of the liquid, and the liquid can be completely liquefied only by increasing the water quantity, so that the capacity is high, the elasticity is high, and the cooling efficiency is high;
6) In addition, even part of SO in the double-row slight-slope shower-drop condenser 3 The gas cannot be liquefied at one time, SO 3 Gas flushableDissolving in acid return pipe; the present invention has the advantages of simple structure, low cost, high efficiency, high safety and reliability, and no pollution 3 Is practical and safe.
Drawings
FIG. 1 shows a sulfuric acid system for producing liquid SO according to the invention 3 Is a practical and safe process flow schematic diagram;
FIG. 2 shows a sulfuric acid system for producing liquid SO according to the invention 3 A structural schematic diagram of a double-row micro-slope shower-drop condenser in the practical and safe process;
wherein, each reference sign is:
1-fuming sulfuric acid circulation tank; 2-a circulation pump; 3-spiral plate cooler; 4-fuming sulfuric acid SO 3 An absorption tower; 5-spiral plate type preheater; 6-SO 3 An evaporator; 7-double-row micro-slope shower-drop type condenser, 71-shower-drop pipe, 72-micro-slope pipeline, 73-water receiving tank, 74-splash-proof water-retaining inclined wing plate; 8-liquid SO 3 And (5) a finished product storage tank.
Detailed Description
The present invention will be described in detail and in detail by way of the following examples, which are not intended to limit the scope of the invention, for better understanding of the invention.
Example 1
Referring to FIG. 1, the present embodiment provides a sulfuric acid system for producing liquid SO 3 The practical and safe process of (3) comprises the following steps:
in the process 1, hot flue gas generated by a sulfuric acid system process enters SO 3 In the evaporator 6, the SO3 evaporator 6 is provided with a heating value for steaming, and the SO is passed through 3 The fuming sulfuric acid SO is introduced after the heat exchange and the temperature reduction of the evaporator 6 3 An absorption tower 4;
in the process 2, the fuming sulfuric acid liquid in the fuming sulfuric acid circulating tank 1 is pumped out by adopting the circulating pump 2 and is circulated in two paths, the first path is conveyed to the spiral plate type cooler 3 for cooling treatment, and the second path is conveyed to the spiral plate type preheater 5 for heating treatment, specifically:
the first path of fuming acid liquid cooled by the spiral plate cooler 3 is conveyed to fuming sulfuric acid SO 3 An absorption tower 4 for absorbing the fuming sulfuric acid SO 3 SO contained in the flue gas in the absorption tower 4 3 The gas, the high-concentration oleum obtained returns to the oleum circulation tank 1, and the oleum circulation tank 1 is supplemented with SO of oleum 3 The content is as follows;
the second path of fuming acid liquid preheated by the spiral plate type preheater 5 is conveyed to SO 3 The evaporator 6 is used for evaporating and separating out pure SO 3 The high-temperature fuming sulfuric acid liquid with reduced concentration after evaporation flows out and passes through a spiral plate type preheater 5 and returns to the fuming sulfuric acid circulating tank 1;
process 3, SO 3 Evaporator 6 is heated to evaporate the pure SO separated from fuming sulfuric acid 3 The gas is introduced into a double-row micro-slope shower-drop condenser 7 for cooling treatment, and all or most of SO is treated 3 The gas is condensed to SO 3 Liquid, self-flowing into liquid SO 3 The product tank 8 obtains the product without condensed SO 3 The gas enters fuming sulfuric acid SO 3 The acid return pipe of the absorption tower is dissolved into fuming sulfuric acid for recycling.
As a technical scheme of the embodiment, as shown in FIG. 1, the SO is used in the process 1 3 The flue gas cooled by the evaporator 6 is introduced into the fuming sulfuric acid SO 3 SO contained in the flue gas is absorbed by fuming sulfuric acid liquid in the absorption tower 4 3 Gas, increasing the concentration of fuming sulfuric acid, and absorbing the flue gas from the fuming sulfuric acid SO 3 The top of the absorption tower 4 is discharged and utilized in the dry absorption process of the sulfuric acid removal system.
In addition, the SO 3 SO evaporated by evaporator 6 3 The cyclone foam remover passing through the top of the cyclone foam remover removes acid foam, the acid foam is recycled, and the ratio of the diameter of an outlet pipe of the cyclone foam remover to the diameter of a cylinder of the cyclone foam remover is 2/7-1/3.
As a technical solution of this embodiment, the SO described in process 2 3 Evaporation and separation of SO in evaporator 6 3 The high-temperature acid liquor after gas is introduced into the spiral plate type preheater 5, and exchanges heat with the low-temperature acid liquor in the spiral plate type preheater 5, so that the temperature is highAnd the warm acid liquid is cooled and then discharged out of the plate-type preheater 5 to enter the fuming sulfuric acid circulation tank 1.
As a technical solution of this embodiment, as shown in fig. 1, the efficiency and the area of the spiral-plate type preheater on the second circulation loop must be sufficient, and in the process 2, the spiral-plate type preheaters 5 are two and arranged in series. The two spiral plate type preheaters 5 which are arranged in series have better heat exchange effect, SO that the self heat is fully utilized, the temperature of the fuming sulfuric acid circulating tank 1 is reduced, and the fuming sulfuric acid SO is removed 3 The temperature of the evaporator 6 is fully raised and then enters SO 3 The evaporator 6 is heated by the hot flue gas of the sulfuric acid system process and then is heated, SO that the boiling point of fuming sulfuric acid can be sufficiently reached to quickly evaporate pure SO 3 The gas is most convenient and energy-saving by fully utilizing the fuming sulfuric acid to circulate self heat exchange and utilizing the sulfuric acid system process hot flue gas heat, and the cost is lowest.
As a technical scheme of the embodiment, in the process 2, a small amount of SO volatilized by the high-concentration oleum in the oleum circulation tank 1 3 The gas is pumped by utilizing the negative pressure of the sulfuric acid production system and is conveyed to SO through a pipeline 3 The gas absorber is used for absorbing treatment to prevent smoke from being generated outside the fuming sulfuric acid circulation tank.
As a technical scheme of the embodiment, SO which is not condensed by the double-row micro-slope shower-drop condenser 7 in the process 3 3 Gas enters the fuming sulfuric acid SO 3 The acid return pipe of the absorption tower 4 is contacted with the fuming sulfuric acid with high concentration in the acid return pipe for absorption, and then flows into the fuming sulfuric acid circulation tank 1 together for recycling.
As a technical scheme of the embodiment, in the process 2, the area and the medium flow rate of the spiral plate type preheater 5 are enough, so that sufficient heat exchange can be realized, and the temperature difference between the two media at the cold side after heat exchange of the spiral plate type preheater 5 is less than 20 ℃.
As a technical scheme of the embodiment, in the process 3, SO which is not condensed 3 Gas in fuming sulfuric acid SO 3 The acid return pipe of the absorption tower 4 is converged between 80 mm and 350mm below the elbow when entering the fuming sulfuric acid circulation tank 1, and is filled with high-concentration fuming sulfur in the acid return pipeThe acid is absorbed and dissolved and then is sent into the fuming sulfuric acid circulation tank 1.
As a preferred technical solution of this embodiment, as shown in fig. 2, the double-row micro-slope shower-drop condenser includes a shower pipe 71, a micro-slope pipe 72 and a water receiving tank 73 sequentially arranged from top to bottom, where the micro-slope pipe 72 is formed by two rows of steel single pipes connected in series to form a gradient of 1-3 ° and continuously descending back and forth, and the area corresponds to the capacity. Preferably, the gradient of the steel single pipeline is 1.5-2.5 DEG, and the upper end inlet of the micro-slope pipeline 72 is connected with the SO 3 The top end of the upper end enclosure of the evaporator 6 and the outlet of the lower end are respectively connected with the liquid SO 3 Finished product storage tank 8 and fuming sulfuric acid SO 3 And an 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 straight pipes adjacent to each other vertically on the micro-slope pipeline 72 is 51-57mm. Preferably, the distance between adjacent upper and lower pipelines is 51mm, SO 3 The pipe spacing of the schematic diagram of the evaporator in the attached figure 2 is larger, so that the actual pipe spacing is small, and the effect that the water sprayed onto each pipe falls down to the outside and the splashing water is less is achieved at the same time of being promoted; the design of single pipeline can make double-row overcurrent medium be the same in size, avoids the flow of each pipe of parallelly connected different, and the troublesome disadvantage of condensation control.
As another preferable solution of this embodiment, the showering liquid recovered in the water receiving tank 73 automatically flows into the circulating pool of the cooling tower or is used for supplementing water to the circulating pool of the cooling tower.
Adopts a double-row micro-slope spray-falling type condenser, is externally sprayed with water, has no pressure and is SO in the condenser 3 Pressurized, SO upon leakage 3 The water leaks outwards, the water can not enter the condenser forever, once the traditional tube-in-tube heat exchanger leaks, the water can not enter SO 3 The violent reaction heating explosion accident occurs in the container storage tank and the pipeline, the problems of immersion corrosion and difficult detection of the microslit of the tube array of the traditional condenser are avoided, the leakage point can be safely and timely found, and once the double-row microslope shower-drop type condenser is exposed, the problem of SO is solved 3 Whether liquid or gas in contact with air produces a white apparent smoke immediately, the treatment can be found very quickly.
In addition, two sides of the double-row micro-slope shower-drop condenser 7 are provided with splash-proof water-blocking inclined wing plates 74 which are vertically distributed at intervals, the splash-proof water-blocking inclined wing plates 74 are horizontally installed, and the splash-proof water-blocking inclined wing plates 74 are obliquely opened towards the outer side. The micro-slope pipeline 72 can be seen through the intervals between the upper and lower spaced splash-proof water retaining inclined wing plates 74, ventilation is not affected, water can be fully recovered while splashing prevention, the double-row micro-slope shower-drop condenser can be completely cooled by water, namely, the water shower-drop temperature is extremely higher than the air cooling effect, the heat transfer coefficient is high, the shower water condition can be directly observed, and the inspection is convenient.
As a technical scheme of the embodiment, two shower and drop pipes 71 are provided, wherein a plurality of evenly distributed water outlet holes are formed in the bottom of each shower and drop pipe 71 along the length direction of the shower and drop pipe 71, the water outlet holes face downwards, the aperture is 5-15mm, and the distance from the water outlet holes to the top of the micro-slope pipeline 72 is 20-40mm; preferably, the aperture of the water outlet hole is 8-12mm, which is 25-32mm from the top of the micro-slope pipeline 72, so that the water outlet size can be seen, all holes can be used for evenly discharging water at the same time, and the shower and drop pipe 71 is provided with a water regulating valve for controlling the size, and part of water outlet can be controlled according to the requirement.
In this embodiment, the SO is provided by a process flow device 3 Evaporator 6, double-row micro-slope shower-drop condenser 7 and liquid SO 3 The level of the finished product storage tank 8 and the fuming sulfuric acid circulation tank 1 gradually decreases, and the SO 3 The liquid realizes self-flow among the process flow devices.
Production of liquid SO in this example 3 The practical and safe process of the system realizes the utilization and the cyclic utilization of the heat of the system with full high efficiency, and the anhydrous dry hot flue gas of the sulfuric acid system is utilized to safely heat SO 3 The evaporator is particularly full in heat exchange by circulating fuming sulfuric acid liquid through improving the heat exchange capacity of the preheater, and particularly, the single-tube double-row shower-drop type condenser is created for condensation, so that the production cost is greatly reduced, the reliability and the safety are improved, and the problem of insufficient evaporation heat and the problem of safety and high efficiency of the condenser are effectively solved.
Example 2
Based on the above example 1, this example provides a sulfuric acid system production liquid according to the process described aboveSO 3 As shown in FIGS. 1 and 2, it mainly comprises a fuming sulfuric acid circulation tank 1, a spiral plate type cooler 3, and fuming sulfuric acid SO 3 Absorption tower 4, spiral plate type preheater 5 and SO 3 An evaporator 6 and a double-row micro-slope shower-drop condenser 7.
In this embodiment, the fuming sulfuric acid circulation tank 1 is connected to the spiral plate cooler 3 and the spiral plate preheater 5 through pipelines by a circulation pump 2 respectively, so as to convey the acid liquor in the fuming sulfuric acid circulation tank to the spiral plate cooler 3 for cooling treatment and to the spiral plate preheater 5 for preheating treatment respectively; the spiral plate type cooler 3 passes through the fuming sulfuric acid SO through a pipeline 3 The absorption tower 4 is connected with the fuming sulfuric acid circulation tank 1 to contact and absorb the cooled acid liquor with the flue gas into high-concentration fuming sulfuric acid, and the high-concentration fuming sulfuric acid flows back to the fuming sulfuric acid circulation tank 1 through an acid return pipe;
in this embodiment, the plate preheater 5 is connected to the SO via a pipe 3 The bottom of the evaporator 6 is used for feeding the preheated acid liquor into the SO 3 The evaporator 6 performs an evaporation process; the SO 3 The side part of the upper end socket of the evaporator 6 is connected with the spiral plate type preheater 5 through a pipeline so as to convey fuming sulfuric acid liquid with reduced concentration after evaporation to the spiral plate type preheater 5 for heat exchange with concentrated acid liquid to be evaporated. The SO 3 The top of the upper end enclosure of the evaporator 6 is connected with the double-row micro-slope shower-drop condenser 7 through a pipeline SO as to evaporate pure SO 3 The gas is conveyed into the double-row micro-slope shower-drop condenser 7 for condensation treatment, and condensed SO 3 Liquid flow into liquid SO through pipeline 3 A finished product storage tank 8; uncondensed SO 3 Gas enters the fuming sulfuric acid SO through a pipeline 3 The acid return pipe of the absorption tower 4 is contacted with the fuming sulfuric acid with high concentration in the acid return pipe for absorption, and then flows into the fuming sulfuric acid circulation tank 1 together for recycling.
In this embodiment, as shown in fig. 2, the double-row micro-slope shower-drop condenser 7 includes a shower pipe 71, a micro-slope pipe 72, and a water receiving tank 73 sequentially arranged from top to bottom, where the micro-slope pipe 72 is formed by two ofThe steel single pipelines which are connected in series to form a gradient of 1-3 degrees and continuously descend back and forth are formed, and the area corresponds to the productivity. Preferably, the gradient of the steel single pipeline is 1.5-2.5 DEG, and the upper end inlet of the micro-slope pipeline 72 is connected with the SO 3 The top end of the upper end enclosure of the evaporator 6 and the outlet of the lower end are respectively connected with the liquid SO 3 Finished product storage tank 8 and fuming sulfuric acid SO 3 And an acid return pipe of the absorption tower 4.
In this embodiment, as shown in fig. 2, the distance between the straight pipes adjacent to each other vertically on the micro-slope pipeline 72 is 51-57mm. Preferably, the distance between adjacent upper and lower pipelines is 51mm, SO 3 The schematic diagram of the evaporator is larger in interval in the attached figure 2, so that the actual interval is small for illustrating the structure, and the water sprayed onto each pipe is less in splashing while being promoted; the design of single pipeline can make double-row overcurrent medium be the same in size, avoids the flow of each pipe of parallelly connected different, and the troublesome disadvantage of condensation control. The water in the water receiving tank 73 flows into a cooling tower of the sulfuric acid process system for circulation or is used as make-up water of the cooling tower.
The embodiment adopts a double-row micro-slope shower-drop condenser, which is externally sprayed with water and has no pressure, and SO in the condenser 3 Pressurized, SO upon leakage 3 The water leaks outwards, the water can not enter the condenser forever, once the traditional tube-in-tube heat exchanger leaks, the water can not enter SO 3 The violent reaction heating explosion accident occurs in the container storage tank and the pipeline, the problems of immersion corrosion and difficult detection of the microslit of the tube array of the traditional condenser are avoided, the leakage point can be safely and timely found, and once the double-row microslope shower-drop type condenser is exposed, the problem of SO is solved 3 Whether liquid or gas in contact with air produces a white apparent smoke immediately, the treatment can be found very quickly.
In addition, two sides of the double-row micro-slope shower-drop condenser 7 are provided with intermittent splash-proof water-blocking inclined wing plates 74, and the length direction of the splash-proof water-blocking inclined wing plates 74 is consistent with the horizontal direction of the gradient direction of the micro-slope pipeline 72. The double-row pipe water wetting condition can be seen through the interval between the upper and lower spaced splash-proof water retaining inclined fin plates 74, ventilation is not affected, water can be fully recovered while splashing prevention, the double-row micro-slope shower-drop condenser 7 can be completely cooled by water, leakage safety is not worried at all, namely, the water shower-drop temperature is extremely high compared with the air cooling effect, the heat transfer coefficient is high, the shower state can be directly observed, and the inspection is convenient.
As a technical scheme of the embodiment, two shower and drop pipes 71 are provided, wherein a plurality of evenly distributed water outlet holes are formed in the bottom of each shower and drop pipe 71 along the length direction of the shower and drop pipe 71, the water outlet holes face downwards, the aperture is 5-15mm, and the distance from the water outlet holes to the top of the micro-slope pipeline 72 is 20-40mm; preferably, the aperture of the water outlet hole is 8-12mm, which is 25-32mm from the top of the micro-slope pipeline 72, so that the water outlet size can be seen, all holes can be used for evenly discharging water at the same time, and the shower and drop pipe 71 is provided with a water regulating valve for controlling the size, and part of water outlet can be controlled according to the requirement.
In this embodiment, the SO is provided by a process flow device 3 Top of evaporator 6, double-row micro-slope shower-drop condenser 7 and liquid SO 3 The level of the finished product storage tank 8 and the fuming sulfuric acid circulation tank 1 gradually decreases, and the SO 3 The liquid realizes self-flow among the process flow devices.
In the embodiment, fuming sulfuric acid is pumped out by a circulating pump to be circulated in two paths, and one path of fuming sulfuric acid SO is removed after the temperature of the fuming sulfuric acid is reduced by the spiral plate type cooler 3 Absorption tower for absorbing SO in flue gas 3 The fuming sulfuric acid concentration is improved; after one path is heated by a spiral plate type preheater, the pure SO is evaporated by the evaporator 3 Gas, pure SO 3 Safe and efficient condensation of gas to prepare SO by using double-row micro-slope shower-drop condenser 3 Liquid, while the evaporator evaporates pure SO 3 The hot fuming sulfuric acid liquid with reduced gas concentration flows out of SO 3 After the evaporator, the heat is fully exchanged by the two-stage spiral preheater and then flows back into the fuming sulfuric acid circulation tank for recycling, so that the system heat recycling is fully and efficiently realized, the production cost is greatly reduced, and the problems of safety and high efficiency of the condenser and insufficient heat evaporation amount are effectively solved.
The above description of the specific embodiments of the present invention has been given by way of example only, and the present invention is not limited to the above described specific embodiments. Any equivalent modifications and substitutions for the present invention will occur to those skilled in the art, and are also within the scope of the present invention. Accordingly, equivalent changes and modifications are intended to be included within the scope of the present invention without departing from the spirit and scope thereof.
Claims (9)
1. Sulfuric acid system production liquid SO 3 The practical safety process of (2) is characterized by comprising the following steps:
in the process 1, dry hot flue gas generated by a sulfuric acid system process is subjected to SO 3 In the evaporator (6) is SO 3 An evaporator (6) for providing a heating value;
step 2, the fuming sulfuric acid liquid after being fully preheated and heated by a spiral plate type preheater (5) is conveyed to SO 3 The evaporator (6) is heated to carry out SO 3 Evaporating, and flowing out SO from the high-temperature fuming sulfuric acid liquid with reduced concentration after evaporation 3 The evaporator (6) returns to pass through the spiral plate type preheater (5) to fully preheat the fuming sulfuric acid to be evaporated, and then flows back to the fuming sulfuric acid circulation tank (1) after being cooled;
process 3, SO 3 The evaporator (6) is heated to evaporate fuming sulfuric acid to separate out pure SO 3 Introducing the gas into a double-row micro-slope shower-drop condenser (7) for condensation treatment, and completely or mostly treating SO 3 The gas is condensed to SO 3 Liquid, self-flowing into liquid SO 3 The finished product storage tank (8) is used for obtaining a product without condensed SO 3 The gas enters fuming sulfuric acid SO 3 An acid return pipe of the absorption tower (4);
the double-row micro-slope shower-drop condenser (7) comprises a shower-drop 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 with the gradient of 1-3 degrees and continuously descending back and forth.
2. The sulfuric acid system of claim 1 for producing liquid SO 3 Is characterized in that in the process 2, the number of the spiral plate type preheaters (5) is two, and the spiral plate type preheaters are arranged in series.
3. The sulfuric acid system of claim 1 for producing liquid SO 3 The practical and safe process is characterized in that in the process 2, the temperature difference between two media at the cold side after heat exchange by the spiral plate type preheater (5) is less than 20 ℃.
4. The sulfuric acid system of claim 1 for producing liquid SO 3 Is characterized in that in process 3, SO which is not condensed 3 Gas in fuming sulfuric acid SO 3 The acid return pipe of the absorption tower is converged between 80 mm and 350mm below an elbow when entering the fuming sulfuric acid circulation tank (1), absorbed and dissolved by high-concentration fuming sulfuric acid in the acid return pipe, and then sent into the fuming sulfuric acid circulation tank (1).
5. The sulfuric acid system of claim 1 for producing liquid SO 3 The practical safety process of the process is characterized in that the distance between the straight pipes adjacent to each other up and down on the micro-slope pipeline (72) is 51-57mm.
6. The sulfuric acid system of claim 5 for producing liquid SO 3 The practical safety process is characterized in that the number of the shower and drop pipes (71) is two, a plurality of evenly distributed water outlet holes are formed in the bottom of each shower and drop pipe (71) along the length direction of the shower and drop pipe, 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 pipeline (72) is 20-40mm.
7. The sulfuric acid system of claim 1 for producing liquid SO 3 The safe process is characterized in that splash-proof water-retaining inclined wing plates (74) are respectively arranged on two sides of the micro-slope pipeline (72), and the length direction of the splash-proof water-retaining inclined wing plates (74) is consistent with the horizontal direction of the micro-slope pipeline (72).
8. The sulfuric acid system of claim 1 for producing liquid SO 3 Is characterized in that the water in the water receiving tank (73) flows into a cooling tower circulation of a sulfuric acid process system or is used as make-up water of the cooling tower.
9. The sulfuric acid system of claim 1 for producing liquid SO 3 The practical and safe process of (2) is characterized in that in the process 3, the process flow equipment SO 3 Evaporator (6), double-row micro-slope shower-drop condenser (7), liquid SO 3 The level of the finished product storage tank (8) and the fuming sulfuric acid circulation tank (1) is gradually reduced, and the SO 3 The liquid realizes self-flow between the process flow equipment.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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