CN1257039A - New technology for synthesizing chlorosulfonic acid - Google Patents
New technology for synthesizing chlorosulfonic acid Download PDFInfo
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- CN1257039A CN1257039A CN 98125479 CN98125479A CN1257039A CN 1257039 A CN1257039 A CN 1257039A CN 98125479 CN98125479 CN 98125479 CN 98125479 A CN98125479 A CN 98125479A CN 1257039 A CN1257039 A CN 1257039A
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Abstract
A technological processf or synthesizing chlorosulfonic acid, belonging to the field of sulfur-bearing, halogen-bearing, hydrogen-containing and oxygen-containing compound technology, is characterized by adding air-supplying, separating and deentrainment step in the course of cooling and drying hydrogen chloride gas in existent technological process, and adding induced draught and buffering step in the course of drying hydrogen chloride gas and making it feed into main and auxiliary reaction towers for reaction, and utilizing the above-mentioned improvement to effectively reduce the acid-carrying and liquid-carrying amount of reaction gas-hydrogen chloride gas so as to raise product yield and quality, and maximally prevent corrosion of equipment and pipeline, and prolong their service life.
Description
The invention belongs to the technical field of compounds containing sulfur, halogen, hydrogen and oxygen, and particularly relates to a novel synthesis process of chlorosulfonic acid.
In the prior art, chlorosulfonic acid (HSO)3Cl) production is generally based on the following reaction: main reaction: (I) sidereaction: (II) The raw material is SO3And hydrogen chloride, reacting the byproduct HS generated in the step (III) in an auxiliary tower2O5Cl2 +And HSO4 -Reaction with hydrogen chloride gas:
after the reaction mixture is condensed, part of SO still remains in the tail gas3、SO2And HCl gas, further 98% H in an acid wash column2SO4Absorbing and treating in a water washing tower to reach the standard and discharging. The flow chart of the conventional production process is shown in figure 1.
In the raw materials of the above synthesis process, SO3It is generally led out of the converter of the sulfuric acid system in a concentration of 7.5-8% (volume ratio). Or preparing SO from burning sulfur and roasting pyrite specially for producing chlorosulfonic acid3A gas; the HCl gas can come from a chlorine and hydrogen synthesis furnace or a Mannheim reaction furnace for producing potassium sulfate, and the H in the HCl gas can be responded2The O content is strictly required. Since large amounts of water-laden HCl gas can severely corrode equipment; in another aspect, HSO3Cl is an extremely unstable strong acid, and decomposes in the presence of water to release a large amount of heat and smoke, which deteriorates the reaction conditions and seriously affects the quality of the finished product. The reaction formula is as follows: (V)
Since the main reaction is a reversible reaction, it is common in industry to increase SO3The method of molecular ratio of HCl and the method of HCl can improve the synthesis rate. In liquid HSO3In Cl, SO3The solubility therein is correspondingly greater than that of HCl, and a slight excess of HCl can generally be controlled.
In the process of producing potassium sulfate by the Mannheim method, 0.4 ton of hydrogen chloride can be produced as a by-product for each ton of potassium sulfate, and for digesting and utilizing the hydrogen chloride gas, CN1165779A discloses a method for directly preparing potassium sulfate by using low-concentration hydrogen chlorideA new process for preparing high-concentration chlorosulfonic acid includes the following steps: cooling high temperature hydrogen chloride gas generated by the Manham furnace, defoaming, dehydrating and drying the hydrogen chloride gas by a washing tower and a drying tower, and mixing the dried hydrogen chloride gas with SO in a second reactor3The gas is fully reacted in gas phase, the reaction product is condensed and separated by a condenser and a separator, and the semi-finished product after separation enters a first reactor to continue to react with HCl gas discharged from a drying tower① in the scheme, because a washing tower is additionally arranged between a cooler and a fan, the water content in the hydrogen chloride gas is increased to become a main reason of liquid carrying of the gas, the liquid carrying of the hydrogen chloride gas firstly influences the reaction and further influences the product quality, secondly, in the gas conveying process, the dilute hydrochloric acid is accumulated in a pipeline to reduce the sectional area of the pipeline, the resistance is increased, the flow and pressure fluctuation of the hydrogen chloride gas are increased, the corrosion of equipment is accelerated due to the existence of water, the service life of the equipment is shortened, ② a fan is additionally arranged between the washer and a drying tower, so that the corrosion of the hydrogen chloride gas to the fan is intensified when the hydrogen chloride gas passes through the fan before drying, the water carrying liquid of the fan can damage the balance of the fan to introduce vibration, the noise is large, the fan is easy to damage, the fan output is reduced quickly, most of the gas from a Manhamm furnace is cooled down to absorb the hydrogen chloride gas to generate hydrochloric acid, the hydrochloric acid becomes one of the reason of the liquid carrying of the chloride, and the water is separated.
The invention aims to provide a novel process for synthesizing chlorosulfonic acid, which can overcome the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: the new chlorosulfonic acid synthesizing process includes the following steps:
a. cooling the high-temperature hydrogen chloride gas from the Mann-Hamm furnace (1) by a cooler (2);
b. drying the gas by a drying tower (5);
c. the dried hydrogen chloride gas enters a main reaction tower (8) to carry out gas phase reaction with the added sulfur trioxide gas;
d. the semi-finished product obtained by the reaction enters an auxiliary reaction tower (11) to continuously react with the hydrogen chloride gas from the drying tower (5) to obtain a finished product;
e. condensing and separating the gas obtained by the reaction through a condenser (9) and a separator (10), carrying out acid washing and water washing on the separated gas through an acid washing tower (12) and a water washing tower (13), and then emptying after reaching the standard;
the invention is characterized in that: a blower (3) is arranged between the step a and the step b for blowing air, and a separation demister (4) is arranged for pre-separating and removing the dilute hydrochloric acid carried in the hydrogen chloride gas; and a draught fan (6) is additionally arranged between the steps b and c for draught.
And a buffer (7) is additionally arranged between the step b and the step c and behind the induced draft fan (6) to stabilize the gas pressure.
In the step a, the hydrogen chloride gas is cooled to 32-80 ℃.
And c, reducing the water content in the hydrogen chloride gas dried in the step b to be below 0.1 percent by weight, wherein the hydrogen chloride gas is in a normal-temperature and normal-pressure state, and the hydrogen chloride content is 20-54 percent by volume.
c SO added in step3The gas content is 7-9% by volume, the temperature is 160-215 ℃, and the reaction temperature is controlled between 150-210 ℃.
In the step d, the reaction temperature in the auxiliary reaction tower (11) is 20-50 ℃.
And e, adopting an unequal channel spiral plate heat exchanger as the condenser in the step e, wherein the width of a gas side channel of the heat exchanger is 10-50mm, and the width of a water side channel of the heat exchanger is 5-30 mm.
FIG. 1 is a flow chart of a conventional chlorosulfonic acid production process;
FIG. 2 is a flow chart of a chlorosulfonic acid production process disclosed in CN 1165779A;
FIG. 3 is a flow chart of the new process for synthesizing chlorosulfonic acid.
In the present invention, the washer is removed from the drying tower and the cooler in the existing chlorosulfonic acid production process, and the separation demister is arranged, so that the water source in the reaction gas is reduced, the water in the hydrogen chloride gas from the Mannheim furnace is removed to the maximum extent, the water content in the reaction gas can be effectively controlled, the side reaction is reduced, the corrosion of dilute hydrochloric acid to equipment is avoided, and the product quality is also improved. The forced draught blower is additionally arranged in front of the cooler and the separation demister, and the induced draft fan is additionally arranged between the drying tower and the auxiliary tower, so that the gas pressure can be increased, the long-distance conveying requirement can be ensured, the gas flow is increased, and the reaction requirement in the main and auxiliary towers can be still ensured even if the content of hydrogen chloride in the gas discharged from the Mannheim furnace is very low. The buffer is arranged between the main and auxiliary towers and the induced draft fan, so that the pressure and the flow of the hydrogen chloride gas are better stabilized, the normal operation of the synthesis reaction is facilitated, and the conversion rate of the raw materials is improved. The spiral plate heat exchanger with unequal channels is used as the condenser, and compared with the traditional condenser such as a calandria condenser, the condenser has the advantages of small occupied area, high heat exchange rate, cooling water saving, few static sealing points, and capability of reducing the maintenance workload. The process has relatively relaxed limitations on the concentration, temperature and water content of the raw material gas, can obtain chlorosulfonic acid with the content of over 98 percent, and meets the national high-grade product requirements.
The invention is further illustrated by the following examples in connection with the accompanying drawings.
Example 1, a new process for the synthesis of chlorosulfonic acid, comprising the following steps:
a. cooling the hydrogen chloride gas from the Mannheim furnace 1 to 60 ℃ by a cooler 2;
a', pre-separating the entrained dilute hydrochloric acid in the cooled hydrogen chloride gas by a blower 3 and a separation demister 4;
b. drying the gas by a drying tower 5, and reducing the water content in the dried hydrogen chloride gas to 0.01 percent by weight, wherein the hydrogen chloride gas is in a normal temperature and normal pressure state, and the hydrogen chloride content is 48 percent by volume;
b', pressurizing the dried hydrogen chloride gas by a draught fan 6, and buffering by a buffer 7 to stabilize the gas pressure;
c. the gas enters a main reaction tower 8 to carry out gas phase reaction with the added sulfur trioxide gas, SO3The gas content is 7.5 percent by volume, the temperature is 182 ℃, and the reaction temperature is 180 ℃;
d. semi-finished product obtained by reaction (liquid HSO)3Cl and unreacted SO3) The hydrogen chloride gas entering the auxiliary reaction tower 8 and coming out of the drying tower 5 continuously react to obtain a finished product, namely liquid HSO3Cl, the reaction temperature is 48 ℃;
e. the gas obtained by the reaction is condensed and separated by a condenser 9, an unequal channel spiral plate heat exchanger and a separator 10, and the separated gas is treated by acidThe washing tower 12 and the washing tower 13 are acid-washed and water-washed to remove SO2、SO2And HCl and the like, and the gas is discharged after reaching the standard.
Example 2, a new process for synthesizing chlorosulfonic acid, in this example, the hydrogen chloride gas in step a was cooled to 45 ℃, the water content in the hydrogen chloride gas after drying in step b was reduced to 0.03% by weight, the hydrogen chloride content was 49% by volume, and the SO in step c was3The gas content was 8.0% by volume, the temperature was 176 ℃, the reaction temperature was 178 ℃, and the reaction temperature in step d was 40 ℃, otherwise the same as in example 1.
Example 3, a new process for synthesizing chlorosulfonic acid, in this example, the temperature of the hydrogen chloride gas in step a was reduced to 68 ℃, the water content in the hydrogen chloride gas after drying in step b was reduced to 0.09% by weight, the hydrogen chloride content was 47% by volume, and the SO in step c was reduced to a level of 47% by volume3The gas content was 7.2% by volume, the temperature was 190 ℃, the reaction temperature in step d was 50 ℃, and the other examples are the same as example 1.
Claims (7)
1. The new chlorosulfonic acid synthesizing process includes the following steps:
a. cooling the high-temperature hydrogen chloride gas from the Mann-Hamm furnace (1) by a cooler (2);
b. drying the gas by a drying tower (5);
c. the dried hydrogen chloride gas enters a main reaction tower (8) to carry out gas phase reaction with the added sulfur trioxide gas;
d. the semi-finished product obtained by the reaction enters an auxiliary reaction tower (11) to continuously react with the hydrogen chloride gas coming out of the drying tower (5) to obtain a finished product;
e. condensing and separating the gas obtained by the reaction through a condenser (9) and a separator (10), carrying out acid washing and water washing on the separated gas through an acid washing tower (12) and a water washing tower (13), and then emptying after reaching the standard;
the invention is characterized in that: a blower (3) is arranged between the step a and the step b for blowing air, and a separation demister (4) is arranged for pre-separating and removing the dilute hydrochloric acid carried in the hydrogen chloride gas; and a draught fan (6) is additionally arranged between the steps b and c for draught.
2. The synthesis process according to claim 1, wherein a buffer (7) is additionally arranged between the steps b and c and after the induced draft fan (6) to stabilize the gas pressure.
3. The process of claim 1 or 2, wherein in step a, the hydrogen chloride gas is cooled to 32-80 ℃.
4. The synthesis process of claim 1 or 2, wherein the water content in the hydrogen chloride gas after drying in step b is reduced to less than 0.1% by weight, and the hydrogen chloride gas is in a normal temperature and pressure state, and the hydrogen chloride content is 20-54% by volume.
5. The process of claim 1 or 2, wherein the SO added in step c is3The gas content is 7-9% by volume, the temperature is 160-215 ℃, and the reaction temperature is controlled between 150-210 ℃.
6. The process according to claim 1 or 2, wherein the reaction temperature in the auxiliary reaction column (11) in step d is 20 to 50 ℃.
7. The synthesis process according to claim 1 or 2, wherein the condenser in the step e adopts an unequal channel spiral plate heat exchanger, the width of a channel on the gas side of the heat exchanger is 10-50mm, and the width of a channel on the water side of the heat exchanger is 5-30 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98125479 CN1257039A (en) | 1998-12-11 | 1998-12-11 | New technology for synthesizing chlorosulfonic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98125479 CN1257039A (en) | 1998-12-11 | 1998-12-11 | New technology for synthesizing chlorosulfonic acid |
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| CN1257039A true CN1257039A (en) | 2000-06-21 |
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| CN 98125479 Pending CN1257039A (en) | 1998-12-11 | 1998-12-11 | New technology for synthesizing chlorosulfonic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105111111A (en) * | 2015-09-10 | 2015-12-02 | 泰兴市臻庆化工有限公司 | Preparation method for aryl sulfonyl chloride derivative |
-
1998
- 1998-12-11 CN CN 98125479 patent/CN1257039A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105111111A (en) * | 2015-09-10 | 2015-12-02 | 泰兴市臻庆化工有限公司 | Preparation method for aryl sulfonyl chloride derivative |
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