CN106800276B - Utilize the industrialized preparing process of sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid - Google Patents
Utilize the industrialized preparing process of sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid Download PDFInfo
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- CN106800276B CN106800276B CN201710186002.8A CN201710186002A CN106800276B CN 106800276 B CN106800276 B CN 106800276B CN 201710186002 A CN201710186002 A CN 201710186002A CN 106800276 B CN106800276 B CN 106800276B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/46—Compounds containing sulfur, halogen, hydrogen, and oxygen
- C01B17/466—Chlorosulfonic acid (ClSO3H)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
A kind of industrialized preparing process using sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid includes the SO in one turn of a, use flue gas3Produce 40% oleum；B, sterling SO is produced in evaporation3Gas；C, hydrochloric acid desorption produces sterling HCl；D, with HCl gas and sterling SO3Gas synthesis crude product chlorosulfonic acid；E, the purification of chlorosulfonic acid；With the processing of f, tail gas.Because of sterling SO3SO is free of in gas2Gas; tail gas is few; be conducive to protect environment, other impurities be free of in sterling, side reaction is reduced; improve product quality; the competitiveness of product in market is improved, large-scale industrial production is able to achieve, and the existing sulfuric acid of leading portion industrial sulphuric acid technique, niacin process units can be made full use of; the exhaust treatment system that industrial sulphuric acid process units is all returned after vent gas treatment, reduces blowdown flow rate.
Description
Technical field
The invention belongs to field of inorganic chemical engineering, are related to a kind of industrialization using sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid
Production method.
Background technique
Chlorosulfonic acid as a kind of important industrial chemicals, be widely used in manufacture sulfonamide, reactive dye, detergent,
Plastics, pesticide and national defense industry raw material etc..Traditional chlorosulfonic acid synthetic method is using HCl, SO3Gas phase synthesis method, raw material
Gas Cl2, H2It burns in HCl synthetic furnace, HCl gas is synthesized, after cooled dehydrated, with SO3Gas mixing is closed into chlorosulfonic acid
At tower, after the gas phase chlorosulfonic acid of synthesis is cooled to liquid, finished pot is flowed into after auxiliary suction tower is further reacted with HCl.Traditional
In chlorosulfonic acid production process, SO3SO is first produced by roasting sulphur or troilite2, SO2SO is obtained through catalysis oxidation3, therefore generated
SO3Mass concentration it is lower, general only 7% or so, not more than 9%.The method is because there are also a large amount of SO in system2Gas
Body and non-reactive inert gas cause synthetic tower, condenser and Environmental-protecting treater sulfuric acid absorption tower, water absorption tower and alkali
Absorption tower it is huge, also result in daily production safeguard complicate, be unfavorable for environment, treating tail gas is costly, while product
The low influence quality of concentration.
Summary of the invention
The present invention is directed to propose a kind of industrialized preparing process using sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid, can obtain
To the chlorosulfonic acid of excellent grade, and it is able to achieve large-scale industrial production.
Device used in this industrialized preparing process using sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid includes niacin
Tower, desorption tower, reboiler, double-effect heat exchanger, sulfur trioxide evaporator, spiral-plate heat exchanger, niacin control valve, niacin circulation
Slot, first condensed in two stages device, chlorosulfonic acid synthetic tower, second condensed in two stages device, auxiliary absorber, demister, cyclonic separation
Device, finished acid delivery valve, finished acid heat exchanger, chlorosulfonic acid finished product geosyncline, water scrubber, pickling tower and HCl scrubbing tower；Its technique mistake
Journey comprises the steps of:
A, 40% oleum is produced: one turn of flue gas of sulfuric acid apparatus is sent into niacin tower, it will in niacin circulating slot
Oleum (referred to as " niacin ") squeezes into the SO in one turn of flue gas of niacin tower cyclic absorption3, improve Nicotinic to 40%,
Flow back to niacin circulating slot；
B, sterling SO3Gas is produced: after the concentration of the niacin in niacin circulating slot reaches 40%, opening niacin control
The niacin of 40% concentration in niacin circulating slot is sent into sulfur trioxide evaporator, is heated, steamed high-purity by low-pressure steam by valve
SO3Gas is sent to chlorosulfonic acid synthetic tower, and the niacin after evaporation passes back into niacin circulating slot；
C, hydrochloric acid desorption produces sterling HCl:31% concentrated hydrochloric acid after double-effect heat exchanger and the heat exchange of the dilute hydrochloric acid at desorption tower bottom
Pump is spilled into tower to desorption tower top through distributor, HCl gas that the dilute hydrochloric acid at desorption tower bottom is generated by reboiler be spilled into
Concentrated hydrochloric acid carries out mass transfer exchange, and desorption tower top obtains the HCl gas containing a small amount of moisture, then after first condensed in two stages device removes water
Obtain the HCl gas that content is greater than 99%；
D, the synthesis of crude product chlorosulfonic acid: above walking obtained HCl gas and enter HCl scrubbing tower, dry through 98% sulfuric acid scrubbing
Afterwards, into chlorosulfonic acid synthetic tower, with the sterling SO from sulfur trioxide evaporator3Gas mixing, by Multi-level deflector plate in tower
It is sufficiently mixed, reacts generation crude product chlorosulfonic acid, enter chlorosulfonic acid finished product geosyncline after second condensed in two stages device condenses；
E, the purification of chlorosulfonic acid: the chlorosulfonic acid in chlorosulfonic acid finished product geosyncline enters auxiliary by pump conveying after heat exchanger cools down
Absorption tower, the reaction was continued with the HCl gas on a small quantity from HCl scrubbing tower, generates chlorosulfonic acid, and reacting rear material is back to chlorosulfonic acid
It is defeated to open finished acid until the product content in chlorosulfonic acid finished product geosyncline is qualified for finished product geosyncline, such cyclic absorption HCl gas
Valve out exports finished product, adjusts and produces sour flow, guarantees that the product content of output is qualified；
F, the processing of tail gas: the uncooled material after second condensed in two stages device enters cyclone separator and demister,
Liquid self-flowing obtained after separation enters chlorosulfonic acid finished product geosyncline, and gas then enters pickling tower, water scrubber processing, finally enters sulphur
Sour device dynamic wave exhaust treatment system is further processed.
Industrialized preparing process using sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid of the invention compared with traditional handicraft,
High-purity sterling sulfur trioxide unstrpped gas is prepared using the method for 40% niacin of evaporation, is prepared with 31% concentrated hydrochloric acid desorption high-purity
The HCl unstrpped gas of degree, then two bursts of unstrpped gases are mixed, reaction is come into full contact with by synthetic tower Multi-level deflector plate, in gas phase
The chlorosulfonic acid for synthesizing and obtaining after refining excellent grade, because of sterling SO3SO is free of in gas2Gas, tail gas is few, is conducive to protection ring
Border, sterling SO3Also other impurities are free of in gas, side reaction reduces, improves product quality, improve the market competition of product
Power is able to achieve large-scale industrial production, and can make full use of the existing sulfuric acid of leading portion industrial sulphuric acid technique, niacin production dress
It sets, the exhaust treatment system of industrial sulphuric acid process units is all returned after vent gas treatment, reduces blowdown flow rate.
Detailed description of the invention
Attached drawing is the flow chart using the industrialized preparing process of sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid.
Specific embodiment
As shown, device packet used in this industrialized preparing process with sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid
Include niacin tower 1, desorption tower 2, reboiler 3, double-effect heat exchanger 4,5, sulfur trioxide evaporator 6, spiral-plate heat exchanger 7, niacin control
Valve 8 processed, 9, first condensed in two stages devices of niacin circulating slot 11,12,13, second condensed in two stages devices of chlorosulfonic acid synthetic tower 14,15,
Auxiliary absorber 16, demister 17, cyclone separator 18, finished acid delivery valve 19, finished acid heat exchanger 20, chlorosulfonic acid finished product
Slot 22, water scrubber 24, water scrubber circulating pump 23, pickling tower 25 and HCl scrubbing tower 26.
There are a sulfur trioxide unstrpped gas import, the oleum outlet of the lower part of niacin tower and cigarette in the middle part of niacin tower 1
The oleum import of sour circulating slot 9 is connected, and the outlet of niacin circulating slot is connected with the import of the spray head on the top of niacin tower,
The outlet of niacin circulating slot also being connected by hot cell import by niacin control valve 8 and spiral-plate heat exchanger 7, spiral-plate heat exchanger
7 exported by hot cell is connected with the import of sulfur trioxide evaporator 6, boil-off gas outlet and the chlorine sulphur of sulfur trioxide evaporator 6
First import of sour 13 lower part of synthetic tower is connected, phegma outlet the adding by spiral-plate heat exchanger 7 of sulfur trioxide evaporator
Hot cell is connected with the phegma import of niacin circulating slot.The tube side import of the second level heat exchanger 4 of double-effect heat exchanger 4,5 is dense salt
The tube side outlet of sour import, the second level heat exchanger 4 of double-effect heat exchanger 4,5 is connected with the concentrated hydrochloric acid import on 2 top of desorption tower, then
The tube side import of boiling device 3 is connected with the liquid outlet on the side wall of 2 lower end of desorption tower, under the tube side import of reboiler 3 and desorption tower 2
The air inlet in portion is connected, and the gas vent at 2 top of desorption tower passes through the tube side of first condensed in two stages device 11,12 and HCl is washed
The import of 26 lower part of tower is connected, the gas vent and the second import phase of 13 lower part of chlorosulfonic acid synthetic tower at 26 top of HCl scrubbing tower
Even, the gas vent at 13 top of chlorosulfonic acid synthetic tower is connected with the tube side import of second condensed in two stages device 14,15, and second two
The liquid outlet of tube side of grade condenser 14,15 is connected with the first import of chlorosulfonic acid finished product geosyncline 22,26 top of HCl scrubbing tower
Gas vent be also connected with the air inlet of 16 lower part of auxiliary absorber, the outlet of chlorosulfonic acid finished product geosyncline 22 and finished acid exchange heat
The tube side import of device 20 is connected, the spray head import phase of the tube side outlet and 16 top of auxiliary absorber of finished acid heat exchanger 20
Even, the liquid outlet of 16 bottom of auxiliary absorber is connected with the second import of chlorosulfonic acid finished product geosyncline 22, finished acid heat exchanger 20
Tube side outlet also connect with finished acid delivery valve 19.The gas vent and whirlwind of the tube side of second condensed in two stages device 14,15
The import of separator 18 is connected, and the liquid outlet of cyclone separator 18 is connected with the first import of chlorosulfonic acid finished product geosyncline 22, rotation
The gas vent of wind separator 18 is connected with the import of demister 17, the liquid outlet and chlorosulfonic acid finished product geosyncline 22 of demister 17
The first import be connected, the gas vent of demister 17 is connected with the gas feed of pickling tower 25, the gas vent of pickling tower 25
It is connected with the gas feed of water scrubber 24, the gas vent of water scrubber 24 is offgas outlet.
As shown, the specific steps of this industrialized preparing process using sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid
It is as follows:
A, 40% oleum is produced: by the SO from sulfuric acid apparatus3Flue gas (one turn of flue gas) is sent into niacin tower 1, cigarette
Niacin in sour circulating slot 9 is squeezed into niacin tower by pump 10, absorbs the SO in one turn of flue gas3, Nicotinic is improved to 40%,
Then niacin circulating slot 9 is flowed back to, remaining flue gas then returns to sulfuric acid apparatus in niacin tower, and the amount into the niacin of niacin tower passes through
One regulating valve is adjusted.
B, sterling SO3Gas is produced: after the concentration of the niacin in niacin circulating slot 9 reaches 40%, opening niacin control
Niacin is sent into sulfur trioxide evaporator 6 after the heating of spiral-plate heat exchanger 7, is heated, steamed by low-pressure steam by valve 8 processed
High-purity SO3Gas is sent to chlorosulfonic acid synthetic tower 13, and the niacin after evaporation passes back into niacin after 7 heat release of spiral-plate heat exchanger
Circulating slot 9 continuously prepares sterling sulfur trioxide in this way.
C, the concentrated hydrochloric acid that hydrochloric acid desorption produces sterling HCl:31% concentration comes out through double-effect heat exchanger 4,5 and 2 bottom of desorption tower
The heat exchange of dilute hydrochloric acid all the way, pump is spilled into tower to the top of desorption tower 2 through distributor after 31% concentrated hydrochloric acid is heated, and is taken off simultaneously
Inhale the another way dilute hydrochloric acid that tower bottom comes out and enter desorption tower by the HCl gas that reboiler 3 generates, with the concentrated hydrochloric acid that is spilled into
The exchange of row mass transfer, improves the concentration of gas phase HCl in tower, obtains the HCl gas containing a small amount of moisture in desorption tower top, then through first
Condensed in two stages device 11,12 obtains the HCl gas that content is greater than 99% after removing water.
D, the synthesis of crude product chlorosulfonic acid: above walking obtained HCl gas and enter HCl scrubbing tower 26, dry with 98% sulfuric acid scrubbing
After dry, into chlorosulfonic acid synthetic tower 13, with the sterling SO from sulfur trioxide evaporator 63Gas mixing is rolled over by multistage in tower
Flowing plate is sufficiently mixed, reacts, and generates crude product chlorosulfonic acid, then enter after second condensed in two stages device 14,15 condenses chlorosulfonic acid at
Product geosyncline 22.
E, the purification of chlorosulfonic acid: the chlorosulfonic acid in chlorosulfonic acid finished product geosyncline 22 is by 21 conveying of pump, by finished acid heat exchanger
Enter auxiliary absorber 16 after 20 coolings, the by-product (HS in the crude product chlorosulfonic acid of generation is reacted in chlorosulfonic acid synthetic tower2O5Cl2 +、HSO4 -) and the reaction was continued for the HCl gas from HCl scrubbing tower 26 on a small quantity, generates chlorosulfonic acid, and reacting rear material is back to chlorine sulphur
Sour finished product geosyncline 22, such cyclic absorption HCl gas, until the product content in chlorosulfonic acid finished product geosyncline is qualified, product content
After qualification, finished acid delivery valve 19 is opened, finished product is sent to the big tank of tank field chlorosulfonic acid, the output of finished product is carried out continuously, and is adjusted
Section produces sour flow, and the product content to guarantee output is qualified.
F, the processing of tail gas: the uncooled material after second condensed in two stages device 14,15 enters cyclone separator 18, then
By demister 17, liquid self-flowing obtained after separation enters chlorosulfonic acid finished product geosyncline 22, and gas then enters pickling tower 25, absorbs
SO in tail gas3, enter back into water scrubber 24 processing, absorb gas in moisture, finally transport at sulfuric acid apparatus dynamic wave tail gas
Reason system is further processed.The sulfuric acid scrubbing of HCl scrubbing tower 26 and pickling tower 25 in same sulfuric acid storage tank, the effect of two towers
Complementation changes the sulfuric acid concentration in sulfuric acid storage tank small, does not have to often replacement, just need to change when only concentration is lower than 95%.
In this industrialized preparing process using sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid, d walks crude product chlorosulfonic acid
Synthesis can 130~200 DEG C at a temperature of carry out, i.e., temperature in chlorosulfonic acid synthetic tower 13 is controlled at 130~200 DEG C；HCL
Gas and pure SO3Gas can enter synthetic tower with the ratio of 1 ︰ (1.05~1.1) by volume；E is walked in the purification of chlorosulfonic acid, temperature
Degree can control the temperature in 50 ± 5 DEG C, that is, auxiliary absorber 16 and control at 50 ± 5 DEG C.
The outlet of heat exchanger 4,11,14 in figure can all install electrical conductivity monitoring device, and set it is chain, if desalted water
Any super 50us/cm of conductivity, the then pneumatic operated valve that desalted water passes through are closed, and desorption tower circulating pump, synthetic tower circulating pump, niacin follow
Ring pump and desalination pump are by stop jumping.The exchanger base pneumatic operated valve that discharges water will automatically turn on and discharge water, and protect chlorosulfonic acid appliance arrangement.
Claims (2)
1. a kind of industrialized preparing process using sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid, it is characterized in that device packet used
Include niacin tower (1), desorption tower (2), reboiler (3), double-effect heat exchanger (4,5), sulfur trioxide evaporator (6), spiral plate heat exchange
Device (7), niacin control valve (8), niacin circulating slot (9), first condensed in two stages device (11,12), chlorosulfonic acid synthetic tower (13),
Two condensed in two stages devices (14,15), auxiliary absorber (16), demister (17), cyclone separators (18), finished acid delivery valve
(19), finished acid heat exchanger (20), chlorosulfonic acid finished product geosyncline (22), water scrubber (24), pickling tower (25) and HCl scrubbing tower
(26)；Its technical process comprises the steps of:
A, 40% oleum is produced: one turn of flue gas of sulfuric acid apparatus being sent into niacin tower, by the niacin in niacin circulating slot
Squeeze into the SO in one turn of flue gas of niacin tower cyclic absorption3, Nicotinic is improved to 40%, niacin circulating slot is flowed back to；
B, sterling SO3Gas is produced: after the concentration of the niacin in niacin circulating slot reaches 40%, niacin control valve is opened, it will
The niacin of 40% concentration in niacin circulating slot is sent into sulfur trioxide evaporator, is heated by low-pressure steam, steams high-purity SO3Gas
Body is sent to chlorosulfonic acid synthetic tower, and the niacin after evaporation passes back into niacin circulating slot；
C, hydrochloric acid desorption is produced sterling HCl:31% concentrated hydrochloric acid and is pumped after double-effect heat exchanger and the heat exchange of desorption tower bottom dilute hydrochloric acid to de-
Tower top is inhaled, is spilled into tower through distributor, the HCl gas that the dilute hydrochloric acid at desorption tower bottom is generated by reboiler and the concentrated hydrochloric acid being spilled into
Mass transfer exchange is carried out, desorption tower top obtains the HCl gas containing a small amount of moisture, then is contained after first condensed in two stages device removes water
Amount is greater than 99% HCl gas；
D, the synthesis of crude product chlorosulfonic acid: above walking obtained HCl gas and enter HCl scrubbing tower, after 98% sulfuric acid scrubbing is dry, into
Enter chlorosulfonic acid synthetic tower, with the sterling SO from sulfur trioxide evaporator3Gas mixing, it is sufficiently mixed by Multi-level deflector plate in tower
It closes, reaction generation crude product chlorosulfonic acid, enters chlorosulfonic acid finished product geosyncline after second condensed in two stages device condenses；
E, the purification of chlorosulfonic acid: the chlorosulfonic acid in chlorosulfonic acid finished product geosyncline is conveyed by pump, and auxiliary is entered after heat exchanger cools down and is inhaled
Receive tower, the reaction was continued with the HCl gas on a small quantity from HCl scrubbing tower, generate chlorosulfonic acid, reacting rear material be back to chlorosulfonic acid at
Product geosyncline, such cyclic absorption HCl gas open finished acid output until the product content in chlorosulfonic acid finished product geosyncline is qualified
Valve exports finished product, adjusts and produces sour flow, guarantees that the product content of output is qualified；
F, the processing of tail gas: the uncooled material after second condensed in two stages device enters cyclone separator and demister, separation
The liquid self-flowing obtained afterwards enters chlorosulfonic acid finished product geosyncline, and gas then enters pickling tower, enters back into water scrubber processing, finally enters
Sulfuric acid apparatus dynamic wave exhaust treatment system is further processed.
2. utilizing the industrialized preparing process of sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid, feature as described in claim 1
For the d walk the synthesis of crude product chlorosulfonic acid 70-105 DEG C at a temperature of carry out, HCL gas and pure SO3Gas is by volume
The ratio of 1 ︰ (1.05~1.1) enters chlorosulfonic acid synthetic tower；In the purification of the e step chlorosulfonic acid, temperature is controlled 50 ± 5
℃。
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| CN109368601B (en) * | 2018-11-23 | 2023-08-01 | 山东凯盛新材料股份有限公司 | Device and method for producing chlorosulfonic acid from m/p-phthaloyl chloride tail gas |
| CN110272027B (en) * | 2019-06-27 | 2024-04-26 | 科洋环境工程（上海）有限公司 | Wet process system and process for waste sulfuric acid |
| CN111320141A (en) * | 2020-03-05 | 2020-06-23 | 浙江巨化股份有限公司硫酸厂 | Production process for synthesizing high-purity chlorosulfonic acid by gas phase circulation method |
| CN111874932A (en) * | 2020-08-12 | 2020-11-03 | 山东昭和新材料科技股份有限公司 | Method for controlling phosphorus content in aluminum fluoride production |
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| JPS5110840B2 (en) * | 1972-02-16 | 1976-04-07 | ||
| DE2730011A1 (en) * | 1977-07-02 | 1979-01-18 | Hoechst Ag | PROCESS FOR THE PRODUCTION OF CHLOROSULPHONIC ACID |
| CN1067961C (en) * | 1997-06-22 | 2001-07-04 | 四平联合化工股份有限公司 | Process for synthesizing chlorosulfonic acid using high-concentration sulfur trioxide |
| CN100491238C (en) * | 2007-03-16 | 2009-05-27 | 天津市勤发化工有限公司 | Method and device for synthesizing chlorosulfonic acid from liquid sulphur trioxide |
| CN101134565B (en) * | 2007-08-31 | 2010-10-20 | 上海海陆昆仑高科技工程有限公司 | New process for preparing chlorosulfonic acid and equipment thereof |
| CN101774549A (en) * | 2010-01-08 | 2010-07-14 | 山东聊城鲁西化工第六化肥有限公司 | Chlorosulfonic acid production process and equipment thereof |
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Effective date of registration: 20191224 Address after: 314201 room 318, building 1, west of Washan Road, south of Zhongshan Road, Ganggang District, Jiaxing City, Zhejiang Province Patentee after: Zhejiang Jiafu New Material Technology Co., Ltd Address before: No. 2288 Jiaxing City, Zhejiang province 314201 Zhapu Zhejiang Jiaxing Port Economic Development Zone, Binhai Avenue Patentee before: Zhejiang Jiahua Energy Chemical Co., Ltd. |
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