CN1067961C - Process for synthesizing chlorosulfonic acid using high-concentration sulfur trioxide - Google Patents
Process for synthesizing chlorosulfonic acid using high-concentration sulfur trioxide Download PDFInfo
- Publication number
- CN1067961C CN1067961C CN97112819A CN97112819A CN1067961C CN 1067961 C CN1067961 C CN 1067961C CN 97112819 A CN97112819 A CN 97112819A CN 97112819 A CN97112819 A CN 97112819A CN 1067961 C CN1067961 C CN 1067961C
- Authority
- CN
- China
- Prior art keywords
- acid
- gas
- sulfur trioxide
- concentration
- sent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Treating Waste Gases (AREA)
Abstract
The present invention provides a method for synthesizing chlorosulfonic acid by taking high concentration sulfur trioxide as raw materials. A synthesis reaction of the high concentration sulfur trioxide and high concentration hydrochloric acid gas is directly carried out, reaction temperature is controlled from 140 to 160 DEG C to produce chlorosulfonic acid gas which is made into chlorosulfonic acid finished products by cooling. The method changes the former traditional concept by only using low concentration sulfur trioxide for preparing the chlorosulfonic acid. The present invention has the advantages of less raw material consumption, little pollution, good product quality, etc.
Description
The present invention relates to a kind of is the method for the synthetic chlorsulfonic acid of raw material with the sulphur trioxide.
Domestic existing tens tame chlorsulfonic acid factories, the technology that adopts is identical with our factory, promptly all adopting the sulphur trioxide with lower concentration is the raw material production chlorsulfonic acid, concrete steps are that the sulfur trioxide gas and the process exsiccant hydrogen chloride gas of lower concentration directly enters reaction tower, reaction rapidly obtains the liquid chlorsulfonic acid through processes such as overcooling, separation again under 130～230 ℃ temperature.The problem that this technology exists is: the one, and seriously polluted, because lower concentration sulphur trioxide unstripped gas itself contains sulfurous gas and other impurity, after the building-up reactions, the tail gas composition is more complicated, various effective ingredients are difficult to Separation and Recovery, the concentration of obnoxious flavour substantially exceeds national standard in the discharge tail gas, the severe contamination surrounding environment.The 2nd, the raw material consumption height, sulfur trioxide content is low in the unstripped gas, makes reaction conversion ratio low, and the emission concentration of sulphur trioxide, sulfurous gas, hydrogen chloride gas is higher in the tail gas, has caused raw material consumption excessive.The 3rd, quality product is relatively poor, and the foreign gas in the unstripped gas sulphur trioxide enters into the chlorsulfonic acid finished product in sulphur trioxide and hydrogenchloride building-up process, reduced the purity of chlorsulfonic acid, and quality product is descended.
It is little to the purpose of this invention is to provide a kind of pollution, and raw material consumption is lower, and what quality product was higher is the processing method of raw material production chlorsulfonic acid with the high-concentration sulfur trioxide.
Base reason of the present invention is to start with from the concentration that improves the sulphur trioxide unstripped gas, before sulphur trioxide unstripped gas and hcl reaction, separate, make isolated sulfur dioxide gas return the sulfuric acid conversion system, guarantee the sulfur trioxide gas of high density and the hydrogen chloride gas precursor reactant of high density, improve transformation efficiency, reduce consuming, reduce emission of harmful substances.
The processing method of chlorsulfonic acid production of the present invention comprises following steps:
1, sends into the nicotinic acid absorption tower after the cooling of lower concentration sulphur trioxide unstripped gas, after absorbing, obtain free sulphur trioxide concentration and be 20～30% oleum, then oleum is sent into the vaporizer desorb, obtain the sulfur trioxide gas of concentration more than 99%, the oleum after the desorb is sent the nicotinic acid absorption tower again back to and is absorbed;
2, will through exsiccant content more than 90% hydrogen chloride gas and 99% above sulfur trioxide gas by molecular ratio 1～1.05: 1 sends into the chlorsulfonic acid synthetic tower, and temperature is controlled at 140～160 ℃, reacts to obtain gaseous chlorine sulfonic acid;
3, gaseous chlorine sulfonic acid when temperature is controlled at 20～25 ℃, can make liquid chlorsulfonic acid through supercooler;
4, the tail gas after sulphur trioxide absorbs is sent sulfuric acid workshop section, trans-utilization again back to.
In the cooled tail gas of gaseous chlorine sulfonic acid, contain obnoxious flavoures such as sulphur trioxide and hydrogenchloride, send into treating column by in the milk of lime and after, enter atmosphere.Acid waste water after the neutralization is squeezed in the carbide slag storage pond, handles with sedimentation in carrying out jointly with carbide slag, and clear liquor is discharged outside the factory.
The present invention makes that the impurity obnoxious flavour in the unstripped gas significantly reduces because the employing high-concentration sulfur trioxide is a raw material, and through the milk of lime neutralizing treatment, the obnoxious flavour that is discharged in the atmosphere significantly reduced than in the past, and concrete data see the following form:
| Sequence number | Title | Unit | Standard | Before the enforcement | After the enforcement |
| 1 | Discharge amount of exhaust gas | m 3/h | 4500 | 50-100 | |
| Nuisance in the waste gas | kg/h | SO 2 22g/m 3 | SO 2 102 | 0 | |
| HCL 1.8g/m 3 | H 2SO 4 134 | 12 | |||
| 4 | |||||
| 3 | Discharge of wastewater | t/h | 20 | 20 | |
| 4 | Nuisance in the waste water | kg/h | SO 2 102 | 0 | |
| H 2SO 4 203 | 108 | ||||
| HCL 140.4 | 74 |
Chlorosulfonic acid production process method of the present invention has in addition also reduced consumption of raw materials, originally produced 880 kilograms of 1 ton of chlorsulfonic acid product consumption of sulfur trioxide according to statistics, adopt producing and manufacturing technique of the present invention only to need 748 kilograms, reduced by 132 kilograms, the annual sulfurous gas that reduces tail row loss is rolled over 2000～3000 tons of sulfuric acid amount.
Describe technological process of the present invention below in detail.
Sulphur trioxide unstripped gas cooling with lower concentration is sent into the nicotinic acid absorption tower later, after absorbing, when free sulphur trioxide concentration reaches 20～30%, this oleum is sent into the vaporizer desorb, obtain the sulfur trioxide gas of concentration more than 99%, the oleum after the desorb is sent the nicotinic acid absorption tower again back to and is absorbed; Hydrogen chloride gas and sulfur trioxide gas are sent into the chlorsulfonic acid synthetic tower by molecular ratio at 1.05: 1, temperature is controlled at 140～160 ℃, and gas-phase reaction obtains the chlorsulfonic acid product, and gaseous chlorine sulfonic acid is through supercooler, when temperature is controlled at 20～25 ℃, can make the chlorsulfonic acid finished product; Contain a large amount of sulfurous gas and sulphur trioxide in the tail gas after sulphur trioxide absorbs, send sulfuric acid workshop section trans-utilization again back to; The later tail gas of gaseous chlorine sulfonic acid cooling send into treating column by in the milk of lime and after, enter atmosphere, neutralization back acid waste water is squeezed in the carbide slag storage pond, in carrying out jointly with carbide slag and sedimentation handle, clear liquor is discharged outside the factory.
Claims (2)
1, a kind of processing method that adopts the synthetic chlorsulfonic acid of high-concentration sulfur trioxide, it is characterized in that: this processing method comprises following steps:
A, the cooling of lower concentration sulphur trioxide unstripped gas are sent into the nicotinic acid absorption tower later, after absorbing, obtain free sulphur trioxide concentration and be 20～30% oleum, then oleum is sent into the vaporizer desorb, obtain the sulfur trioxide gas of concentration more than 99%, desorb after-fume sulfuric acid is sent the nicotinic acid absorption tower again back to and is absorbed;
B, will be through exsiccant hydrogen chloride gas and concentration the sulfur trioxide gas more than 99% by molecular ratio 1～1.05: 1 sends into the chlorsulfonic acid synthetic tower, and temperature is controlled at 140～160 ℃, and gas-phase reaction obtains chlorsulfonic acid;
C, gaseous chlorine sulfonic acid when temperature is controlled at 20～25 ℃, can make the liquid chlorsulfonic acid through supercooler;
Tail gas after D, sulphur trioxide absorb is sent sulfuric acid workshop section, trans-utilization again back to.
2, the processing method of the synthetic chlorsulfonic acid of employing high-concentration sulfur trioxide according to claim 1, it is characterized in that: this processing method also comprises following steps: promptly
The later tail gas of gaseous chlorine sulfonic acid cooling send into treating column by in the milk of lime and after, enter atmosphere; Acid waste water after the neutralization is squeezed in the carbide slag storage pond, handles with sedimentation in carrying out jointly with carbide slag, and clear liquor is discharged outside the factory.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97112819A CN1067961C (en) | 1997-06-22 | 1997-06-22 | Process for synthesizing chlorosulfonic acid using high-concentration sulfur trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97112819A CN1067961C (en) | 1997-06-22 | 1997-06-22 | Process for synthesizing chlorosulfonic acid using high-concentration sulfur trioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1203188A CN1203188A (en) | 1998-12-30 |
| CN1067961C true CN1067961C (en) | 2001-07-04 |
Family
ID=5172485
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97112819A Expired - Fee Related CN1067961C (en) | 1997-06-22 | 1997-06-22 | Process for synthesizing chlorosulfonic acid using high-concentration sulfur trioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1067961C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800276B (en) * | 2017-03-27 | 2018-12-21 | 浙江嘉化能源化工股份有限公司 | Utilize the industrialized preparing process of sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid |
| CN109651206A (en) * | 2019-01-14 | 2019-04-19 | 杭州海虹精细化工有限公司 | A method of chlorosulfonation is carried out using sulfur trioxide |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5110840B2 (en) * | 1972-02-16 | 1976-04-07 | ||
| EP0071133A2 (en) * | 1981-07-29 | 1983-02-09 | Bayer Ag | Process for preparing chlorosulfonic acid |
| JPS5855313A (en) * | 1981-09-29 | 1983-04-01 | Nippon Soda Co Ltd | Manufacture of chlorosulfonic acid |
-
1997
- 1997-06-22 CN CN97112819A patent/CN1067961C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5110840B2 (en) * | 1972-02-16 | 1976-04-07 | ||
| EP0071133A2 (en) * | 1981-07-29 | 1983-02-09 | Bayer Ag | Process for preparing chlorosulfonic acid |
| JPS5855313A (en) * | 1981-09-29 | 1983-04-01 | Nippon Soda Co Ltd | Manufacture of chlorosulfonic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1203188A (en) | 1998-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4053507A (en) | Method of recovering unreacted materials and heat in urea synthesis | |
| CN101006011A (en) | Method for producing a fertilizer containing urea and ammonium sulphate | |
| US4539077A (en) | Process for the preparation of urea | |
| CN1939840A (en) | Tail gas treatment and reutilization for calcium carbide stove | |
| CN211521596U (en) | System for preparing analytically pure sulfuric acid from smelting flue gas | |
| CN111115587A (en) | Method and system for preparing analytically pure sulfuric acid from smelting flue gas | |
| CN101327931A (en) | Silica gel cleaning production method and sulfuric acid production method | |
| CN101653688B (en) | Process flow for removing CO2 and H2S in gas mixture | |
| CN1067961C (en) | Process for synthesizing chlorosulfonic acid using high-concentration sulfur trioxide | |
| CN110790235B (en) | Comprehensive utilization method of fluorine-containing potassium chloride as organic synthesis byproduct | |
| CN108261913B (en) | Magnesium oxide semi-dry desulfurization process | |
| EP1024136B1 (en) | A process for producing dimethyl sulphoxide | |
| CN1034904A (en) | The method of purifying coke oven gas and getting ammonium hydrogen carbonate as by-product | |
| DE69213342T2 (en) | Process and apparatus for the industrial production of chlorine | |
| CN1554643A (en) | Method and apparatus for improving industrial producing urea | |
| CN201101938Y (en) | Completely recycling system for hydrogen chloride in industry gas | |
| CN218944751U (en) | Coal-fired flue gas treatment system | |
| CN213865389U (en) | System for utilize cement kiln tail waste gas and ardealite preparation ammonium sulfate | |
| CN111097273B (en) | Method and device for treating FCC (fluid catalytic cracking) regenerated flue gas | |
| CN112225228B (en) | Method and system for preparing ammonium sulfate by using cement kiln tail waste gas and phosphogypsum | |
| CN210065171U (en) | Chlorosulfonic acid production system | |
| CN1425487A (en) | Method for single stage circulation absorbing nitrogen oxide intail gas by dilute nitric acid | |
| CN100491238C (en) | Method and device for synthesizing chlorosulfonic acid from liquid sulphur trioxide | |
| JPH0621004B2 (en) | Chlorine dioxide manufacturing method | |
| CN1012357B (en) | Method for recovery of cyanide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Applicant after: Siping Union Chemical Plant, Siping Applicant before: Siping General Union Chemical Plant, Zhonghua |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: SIPING GENERAL UNION CHEMICAL PLANT, ZHONGHUA TO: SIPING COMBINED CHEMICAL CO., LTD. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |