CN1041307C - Method and equipment for preparing sulfate by burning brimstone in dry air - Google Patents
Method and equipment for preparing sulfate by burning brimstone in dry air Download PDFInfo
- Publication number
- CN1041307C CN1041307C CN92106763A CN92106763A CN1041307C CN 1041307 C CN1041307 C CN 1041307C CN 92106763 A CN92106763 A CN 92106763A CN 92106763 A CN92106763 A CN 92106763A CN 1041307 C CN1041307 C CN 1041307C
- Authority
- CN
- China
- Prior art keywords
- sulfate
- methyl
- dry air
- tower
- sulfur
- 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.)
- Revoked
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method and a device for preparing sulfuric acid ester by burning sulfur in dry air. The present invention is characterized in that the device is composed of a blower fan, a freezing-zeolite absorption device, a sulfur burner, a conversion tower, an absorption tower, an etherification tank, an esterification tank, etc. Precooled dry air reacts with burning sulfur so as to prepare dry sulfur dioxide gas which is subsequently converted into 9 to 11% of sulfur trioxide gas, and dimethyl sulfate is used as an absorption solvent and is esterified with dimethyl ether to prepare dimethyl sulfate. The yield and the quality of the device are the same as that of the prior art, raw material consumption is saved by 8/9, transportation amount is saved by 15/16, cost per ton is reduced by 1/7, and the device has obvious economical and social benefits.
Description
The present invention relates to the preparation of Organic Chemicals, particularly a kind of method and apparatus of improved dry air combustion sulphur system methyl-sulfate.
The conventional production methods of methyl-sulfate is to continue to use oleum---the methyl alcohol method, be about to the oleum heating, and make the dme that sulphur trioxide is overflowed and methyl alcohol generates reaction wherein make the methyl-sulfate product.
The maximum deficiency of this method is:
Traffic capacity is big, and cost height-methyl-sulfate per ton need be transported about 3 tons of oleum, and 98% spent acid of generation need transport again more than 2 tons, increases two kinds of transportations on foot, so the expense of sulphur trioxide is big, accounts for 1/3rd of methyl-sulfate cost.
CN 86 1 05064.9 has done improvement to this, and the lower concentration sulphur trioxide that uses the converter of sulphuric acid process to draw is raw material, makes the methyl-sulfate of industrial value after the solvent enrichment.
But this method is defectiveness also,
1. need depend on gas washing in SA production factory, can not self-organizing system, inconvenience user is nearby founded the factory, and methyl-sulfate often needs way far away transportation, increases cost equally;
2. gas washing in SA production is generally made raw material with sulfurous iron ore at present, and detrimental impurity such as arsenic, fluorine influences the quality product of methyl-sulfate in the ore deposit;
3. wherein, sulfurous gas exsiccant traditional technology is, makes it pass through the vitriol oil, removes wherein moisture content with suction, and so, need consume a large amount of vitriol oils every day, and produce a large amount of dilute sulphuric acids, is irrational economically.
Purpose of the present invention is exactly the improvement to above-mentioned prior art, wish to find out a kind of production self-organizing system that makes methyl-sulfate, be convenient to that user nearby founds the factory, guarantee that product is not influenced by detrimental impurity such as arsenic, fluorine, realization anacidity drying operation, lower-cost industrial method and equipment are to overcome all drawbacks of prior art.
The objective of the invention is to be achieved through the following technical solutions:
Will be in advance through freezing, the dry sulfur dioxide gas that exsiccant air and the effect of incendiary sulphur make changes into 9～11% sulfur trioxide gas again, makes lyosorption with methyl-sulfate, through double tower absorbing enriched sulphur trioxide, prepare methyl-sulfate with the dme esterification again.
Design a kind of equipment of dry air combustion sulphur system methyl-sulfate, by blower fan, brimstone furnace, formations such as converter, absorption tower, etherificate jar and esterification jar is characterized in that one group of brine freezing device of adjunction---zeolite adsorption system before brimstone furnace.
The equipment of above-mentioned dry air combustion sulphur system methyl-sulfate, it is characterized in that this brine freezing device---zeolite adsorption system, be meant that interchanger, zeolite adsorption tower and connecting tube therebetween by the icy salt solution cooling constitute, the blower fan outlet connects recuperative heat exchanger tube side inlet, the tube side outlet connects the adsorption tower inlet, and the dry air of being derived by the adsorption tower outlet feeds brimstone furnace.
The method of above-mentioned dry air combustion sulphur system methyl-sulfate, it is characterized in that in advance through freezing, exsiccant air, the air that is meant the system of entering earlier through icy salt solution be refrigerated to≤0 ℃, remove most of moisture content in the air, again through zeolite molecular sieve absorption, make wherein that moisture content is reduced to≤0.2g/m
3After enter combustion sulphur chamber.
700～1000 ℃ of combustion sulphur chamber controlled temperature, generate the exsiccant sulfur dioxide gas and import converter, under vanadium catalyst catalysis, 400～600C generates sulphur trioxide, transformation efficiency 98%, sulphur trioxide concentration can reach 9～11%, helping the production of methyl-sulfate, be higher than that CN 86 1 05064.9 provides, also is that contact acid production routine reaches, convertor outlet sulphur trioxide concentration only is 7% the highest 9% level, and unconverted sulfurous gas usually≤0.3%.
Sulphur trioxide is made solvent with methyl-sulfate, absorbs to saturated through double tower pump circulation spray, generates methyl-sulfate with the dme that is made by methyl alcohol in the reaction of esterification jar.
The method of above-mentioned dry air combustion sulphur system methyl-sulfate, the temperature of esterification is 50～100 ℃ when it is characterized in that preparing methyl-sulfate.
Remaining small amounts of sulfur dioxide, sulphur trioxide and the Determination of Trace Sulfur dimethyl phthalate carried secretly in the gas phase absorb through last health tower ammonia process, are converted into the nonhazardous gas emptying, and each harmful substance contents all is lower than legal emission standard in the tail gas.
The present invention is the improvement to traditional processing technology, and its advantage is:
Manufactured and designed a kind of production self-organizing system that makes methyl-sulfate, be convenient to that user nearby founds the factory: detrimental impurity such as no arsenic, fluorine influence quality product; Realized the anacidity drying operation, lower-cost industrial method and equipment have been realized the goal of the invention of expection preferably.
Compared with the prior art, the raw material usage quantity is original 1/9th, and traffic capacity is ten original sixths, reduce the round transport amount, reduce cost 1/7th except that per ton, make outside our factory's remarkable in economical benefits, and remarkable social benefit and indirect economic effect are arranged.
The present invention is further elaborated below in conjunction with drawings and Examples:
Fig. 1 is a Processes and apparatus schematic flow sheet of the present invention.
Among the figure, (1) is blower fan, can adopt roots blower etc.: (2) are recuperative heat exchangers, for example can use shell and tube heat exchanger; (3) be zeolite molecular sieve; (4) be brimstone furnace, horizontal, sulphur adds from its top quantitative ratio, lights, and the exsiccant air feeds from an end quantitative ratio, and the dry sulfur dioxide gas that oxidation generates is guided (5) into from the other end; (5) be converter, routinely the filling vanadium catalyst; (6) be the two-stage absorption tower, beat methyl-sulfate with pump and make lyosorption that the pump circulation countercurrent spray absorbs to saturated; (7) be the health tower, beat ammoniacal liquor with pump and make lyosorption that the pump circulation countercurrent spray absorbs the methyl-sulfate that small amounts of sulfur dioxide, sulphur trioxide and trace in the tail gas are carried secretly, emptying tail gas reaches discharging standards; (8) be the methyl alcohol header tank; (9) be the etherificate jar; (10) be the esterification jar.Wherein, the gas washing in SA production of tower, pump and prior art is similar: the methyl-sulfate of jar, groove and prior art is produced similar.
[embodiment one]
Manufacture and design a cover methyl-sulfate production unit by accompanying drawing.Wherein, (1) is the roots blower of L48 * 66WD-J model, and (2) are 30m
2Shell and tube heat exchanger; (3) be zeolite molecular sieve, the zeolite model is JMT-1; (4) be brimstone furnace, horizontal, φ 1200 * 8000mm, material stainless steel; (5) be converter, routinely the filling vanadium catalyst; (6) be the two-stage absorption tower; (7) be the health tower; Tower, pump are stainless; Emptying place of health tower is apart from ground 30m, and (8) are carbon steels, and (9), (10) all are glass-lined reactors that conventional belt stirs.
Per hour drop into sulphur 150kg, air quantity 25m
3/ min, air moisture content 0.15g/m
3, 700～1000 ℃ of brimstone furnace temperature controls, 400～600 ℃ of converter controlled temperature detect, outlet SO
3Concentration is 11%, unconverted SO
2Content is 0.15%, SO
3Absorb to free amount 25% with methyl-sulfate, feed dme again in 60～100 ℃ of esterifications, distill finished product 500kg, content 98.5%, acidity≤0.5%, productive rate is higher than prior art, quality meets industry standard, and cost reduces by 1/7th than prior art.
[embodiment two]
Manufacture and design a cover methyl-sulfate production unit by accompanying drawing.Wherein, (1) is the roots blower of L41 * 49WD-I model, and (2) are 25m
2Shell and tube heat exchanger; (3) be zeolite molecular sieve, model is FNG-1; (4) be brimstone furnace, horizontal, φ 1000 * 7000mm, material stainless steel; (5)～(10) all with embodiment one.
Per hour drop into sulphur 120kg, air quantity 20m
3/ min, air moisture content 0.18g/m
3, 700～850 ℃ of brimstone furnace temperature controls, 420～560 ℃ of converter controlled temperature detect, outlet SO
3Concentration is 9%, unconverted SO
2Content is 0.2%, SO
3Absorb to free amount 22% with methyl-sulfate, feed dme again in 50～90 ℃ of esterifications, distill finished product 400kg, content 98.3%, acidity≤0.5%, productive rate is higher than prior art, quality meets industry standard, and cost reduces by 1/7th than prior art.
Claims (2)
1. the method for dry air combustion sulphur system methyl-sulfate is characterized in that:
In advance through be refrigerated to≤0 ℃, again through zeolite adsorption to moisture content≤0.2g/m
3Dry air, make the exsiccant sulfur dioxide gas with the effect of incendiary sulphur, change into 9～11% sulfur trioxide gas again,
Make lyosorption with methyl-sulfate, to free amount 22～25%, prepare methyl-sulfate with the dme esterification through double tower absorbing enriched sulphur trioxide again, the temperature of esterification is 50～100 ℃.
2. equipment according to the described dry air of claim 1 combustion sulphur system methyl-sulfate, constitute by blower fan, brimstone furnace, converter, absorption tower, etherificate jar and esterification jar, it is characterized in that the brine freezing that adjunction is made of interchanger, zeolite adsorption tower and connecting tube therebetween before brimstone furnace-zeolite adsorption system, the blower fan outlet connects recuperative heat exchanger tube side inlet, the tube side outlet connects the adsorption tower inlet, and the adsorption tower outlet connects brimstone furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92106763A CN1041307C (en) | 1992-10-24 | 1992-10-24 | Method and equipment for preparing sulfate by burning brimstone in dry air |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92106763A CN1041307C (en) | 1992-10-24 | 1992-10-24 | Method and equipment for preparing sulfate by burning brimstone in dry air |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1086209A CN1086209A (en) | 1994-05-04 |
| CN1041307C true CN1041307C (en) | 1998-12-23 |
Family
ID=4942400
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92106763A Revoked CN1041307C (en) | 1992-10-24 | 1992-10-24 | Method and equipment for preparing sulfate by burning brimstone in dry air |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1041307C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116903497B (en) * | 2023-09-11 | 2024-03-29 | 南京为先科技有限责任公司 | Method for preparing sulfonate surfactant by sulfur trioxide film sulfonation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3536446A (en) * | 1967-09-26 | 1970-10-27 | Chemical Construction Corp | Production of sulfuric acid |
-
1992
- 1992-10-24 CN CN92106763A patent/CN1041307C/en not_active Revoked
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3536446A (en) * | 1967-09-26 | 1970-10-27 | Chemical Construction Corp | Production of sulfuric acid |
Non-Patent Citations (1)
| Title |
|---|
| 精细有机化学品技术手册，上册 第一版 1991.7.1 科学出版社 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1086209A (en) | 1994-05-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3944401A (en) | Process for the removal of gaseous impurities from the exhaust gases of a contact-process plant for the production of sulfuric acid | |
| CN102838096B (en) | Joint production method and production device of dilute nitric acid and concentrated nitric acid | |
| CN101735045B (en) | Method for producing ethyl acetate by using entrainer | |
| CN1864812A (en) | A nitric oxides (NOX) waste pollution control in industrial process and resource reclaiming method | |
| CN109264674A (en) | A kind of technique and system using flue gas during smelting extracting sulfuric acid | |
| CN211521596U (en) | System for preparing analytically pure sulfuric acid from smelting flue gas | |
| JPH09507208A (en) | Reactor, plant and method for sulfuric acid production | |
| CN1041307C (en) | Method and equipment for preparing sulfate by burning brimstone in dry air | |
| CN106800276A (en) | Using the industrialized preparing process of sterling sulfur trioxide vapor- phase synthesis chlorosulfonic acid | |
| CN101020570A (en) | Production process of eliminating simple substance sulphur from SO2 gas | |
| US3849541A (en) | Process for purifying fumes | |
| US4062928A (en) | Process for the preparation of nitric acid | |
| US5389354A (en) | Process for the production of oleum and sulfuric acid | |
| CN1792796A (en) | Process for recoverying cyanuric acid three wastes | |
| CA1069675A (en) | Nitrogen oxide conversion process | |
| CN105502308A (en) | Waste sulfuric acid treatment method | |
| CN212151639U (en) | System for continuous production of sodium thiocyanate and by-product ammonium sulfate by cracking furnace gas | |
| CN1021809C (en) | Industrial manganese sulphate production method | |
| CN204746062U (en) | Hydrogen sulfide desorption system based on photochemical fog ization bed | |
| EP3140253B1 (en) | Process and plant for the production of sulfuric acid | |
| US4148868A (en) | Process for separating SO2 from a current of gas containing the same | |
| CN203612956U (en) | Low-temperature waste heat recovery system used in pyrite and smelting exhaust gas acid preparing device | |
| CN109850855A (en) | A kind of production process and equipment of the concentrated sulfuric acid | |
| CN109052332B (en) | Method for preparing chlorosulfonic acid by regenerating high-COD (chemical oxygen demand) saline dilute acid | |
| CN1272489A (en) | Method for extracting dimethyl sulfate by using sulfur as initiation raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| 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 | ||
| C28 | Revocation of patent right or utility model | ||
| RW01 | Full revocation of patent right |
Decision date of revocation: 20020928 |