CN102515209A - Method for preparing industrial-grade sodium pyrosulfite from tail gas generated in production of acyl chloride - Google Patents
Method for preparing industrial-grade sodium pyrosulfite from tail gas generated in production of acyl chloride Download PDFInfo
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- CN102515209A CN102515209A CN2011104063364A CN201110406336A CN102515209A CN 102515209 A CN102515209 A CN 102515209A CN 2011104063364 A CN2011104063364 A CN 2011104063364A CN 201110406336 A CN201110406336 A CN 201110406336A CN 102515209 A CN102515209 A CN 102515209A
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- sodium pyrosulfite
- tail gas
- acyl chlorides
- produced
- solution
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Abstract
The invention relates to a method for preparing industrial-grade sodium pyrosulfite from tail gas generated in production of acyl chloride. According to the invention, since tail gas generated in production of acyl chloride enters into an absorption tower after rinsing and absorption with a NaCO3 solution, a purification rate of the tail gas is as high as 99%, and SO2 in the tail gas is used as a raw material for production of sodium pyrosulfite, thereby changing the waste into the valuable. The method comprises the following steps: (1) rinsing the tail gas generated in production of acyl chloride so as to remove HCl gas in the tail gas; (2) absorbing SO2 in the treated tail gas by using the NaCO3 solution with a concentration of 150 to 180 g/L so as to obtain slurry containing sodium pyrosulfite; (3) centrifuging the slurry containing sodium pyrosulfite prepared in step (2) so as to obtain a wet sodium pyrosulfite material and liquid; and (4) drying the wet sodium pyrosulfite material obtained in step (3) so as to obtain a finished product of sodium pyrosulfite.
Description
Technical field
The present invention relates to a kind of method for preparing Sodium Pyrosulfite, particularly relate to a kind of acyl chlorides that utilizes and produce the method that tail gas prepares Sodium Pyrosulfite.
Background technology
The normal R-COOH+SOCl that adopts in the acyl chlorides production process
2→ R-COCl+SO
2+ HCl, main exhaust pollutant are SO
2With HCl gas.In order to protect environment not contaminated, need be to HCl gas and SO
2Effectively handle.At present, HCl gas mainly adopts water to absorb and produces hydrochloric acid; SO
2Then adopt in the soda-lime and the preparation calcium sulfite, but this method absorption rate of sulfur dioxide is not high, and the calcium sulfite use that generates is also little.
Summary of the invention
The technical problem that the present invention will solve provides a kind of acyl chlorides that utilizes and produces the method that tail gas prepares the technical grade Sodium Pyrosulfite.
A kind of acyl chlorides that utilizes is produced the method that tail gas prepares the technical grade Sodium Pyrosulfite, may further comprise the steps:
(1) acyl chlorides is produced tail gas through washing, removes HCl gas wherein;
(2) acyl chlorides handled of step (1) is produced tail gas and is used the Na of concentration as 150-180g/L
2CO
3Solution absorption SO
2, the acyl chlorides that step (1) was handled is produced tail gas and Na
2CO
3The liquid that solution reaction obtains is called slurries, and when slurry color when white and pH value is 3.5-4.5 by xanthochromia, absorption reaction is reached home, and obtains containing the slurries of Sodium Pyrosulfite;
(3) slurries that contain Sodium Pyrosulfite that step (2) made are centrifugal, obtain Sodium Pyrosulfite wet feed and liquid, and gained liquid is called mother liquor;
(4) the Sodium Pyrosulfite wet feed that step (3) is obtained obtains the Sodium Pyrosulfite finished product through super-dry.
The acyl chlorides that step (1) was handled is produced tail gas and is used Na
2CO
3Solution absorbs the reaction process that generates Sodium Pyrosulfite and is divided into four-stage:
(1) logical people SO in the sodium carbonate solution of 150-180g/L
2To pH be 3.5-4.5, generate sodium sulfite solution, reaction formula is following:
Na
2CO
3+2SO
2+H
2O＝2NaHSO
3+CO
2；
(2) add again in the gained sodium sulfite solution yellow soda ash to pH be 7～8, make sodium sulfite solution be converted into S-WAT, reaction formula is:
Na
2CO
3+2NaHSO
3＝2Na
2SO
3+CO
2+H
2O；
(3) S-WAT again with SO
2React to pH and reach 3.5-4.5, generate sodium sulfite solution again, its reaction formula is:
Na
2SO
3+SO
2+H
2O＝2NaHSO
3；
4) when solution Central Asia sodium sulphate content reaches supersaturation concentration, separate out the Sodium Pyrosulfite crystallization, reaction formula is following:
2NaHSO
3＝Na
2S
2O
5+H
2O；
This 4 step reaction net reaction is:
Na
2CO
3+2SO
2＝Na
2S
2O
5+CO
2；
This reaction process can experience variation and the reaction solution change in color of reaction solution pH, and the pH of reaction solution rises to 7-8 by 3.5-4.5 earlier, reduces to 3.5-4 by 7-8 again; Simultaneously the reaction solution color also changes thereupon, and along with the rising of pH, reaction solution was become pale yellow again to deep yellow by white before this, afterwards along with the decline of pH, the color of reaction solution also by Huang in vain.So need changing through colour-change and pH, reaction process monitors.
The present invention utilizes acyl chlorides to produce the method that tail gas prepares the technical grade Sodium Pyrosulfite, and the temperature of wherein said Na2CO3 solution is 43-47 ℃.
The present invention utilizes acyl chlorides to produce the method that tail gas prepares the technical grade Sodium Pyrosulfite, and the acyl chlorides that wherein said step (1) was handled is produced tail gas and used Na
2CO
3Solution absorption SO
2Be to adopt three grades of alkali lye to absorb.Three grades of alkali lye absorb equipment therefor and comprise first reaction kettle, second reaction kettle, the 3rd reaction kettle and absorption tower, and first to the 3rd reaction kettle, absorption tower link to each other through pipeline in order, and Na all is housed in each reaction kettle
2CO
3Solution, the acyl chlorides that step (1) was handled is produced tail gas and is fed first reaction kettle and Na
2CO
3Solution reaction, the SO that first reaction kettle fails to sponge
2, get into second and third reaction kettle through pipeline and carry out the absorption of two steps, absorb the tail gas of handling through three grades of alkali lye and enter the people absorption tower again through emptying after the alkali cleaning.Na in the reaction kettle
2CO
3Solution and SO
2Reaction generates slurries, when slurries Central Asia sodium sulphate content reaches supersaturation concentration; Separate out the Sodium Pyrosulfite crystallization, from first reaction kettle, emit slurries, first reaction kettle reduces slurries and is replenished by second reaction kettle; Second reaction kettle is replenished by the 3rd reaction kettle, with the Na for preparing
2CO
3Solution replenishes in the 3rd reaction kettle.
The present invention utilizes acyl chlorides to produce the method that tail gas prepares the technical grade Sodium Pyrosulfite, and wherein white and pH value is 4.0 o'clock to slurry color described in the step (2) by xanthochromia, and absorption reaction is reached home.
The present invention utilizes acyl chlorides to produce the method that tail gas prepares the technical grade Sodium Pyrosulfite, and wherein mother liquor is used for preparing once more Na described in the step (3)
2CO
3Solution.
The beneficial effect that the present invention utilizes acyl chlorides production tail gas to prepare the method for technical grade Sodium Pyrosulfite is: (1) is because acyl chlorides is produced tail gas through washing and Na
2CO
3Get into the absorption tower after the solution absorption, make purification rate that acyl chlorides produces tail gas up to 99%, and adopt soda-lime to absorb SO
2The back gets into the absorption tower, and the purification rate that acyl chlorides is produced tail gas is 81%; (2) acyl chlorides is produced the SO in the tail gas
2As the raw material that Sodium Pyrosulfite is produced, turn waste into wealth.
Below in conjunction with accompanying drawing the present invention is described further.
Description of drawings
Fig. 1 produces the schema that tail gas prepares the method for technical grade Sodium Pyrosulfite for the present invention utilizes acyl chlorides.
Embodiment
Embodiment 1
(1) acyl chlorides is produced tail gas through washing, removes HCl gas wherein;
(2) acyl chlorides handled of step (1) is produced tail gas with 150g/L, 43 ℃ Na
2CO
3Solution carries out three grades of alkali lye and absorbs, and the acyl chlorides that step (1) was handled is produced tail gas and fed first reaction kettle and Na
2CO
3Solution reaction is along with SO
2Absorption, slurry color is pale yellow to deep yellow by leucismus, again by deep yellow shoal yellow in vain; When slurry color when white and pH value is 3.5 by xanthochromia, absorption reaction is reached home, and obtains containing the slurries of Sodium Pyrosulfite; From first reaction kettle, emit the slurries that contain Sodium Pyrosulfite; The slurries that first reaction kettle reduces are replenished by second reaction kettle, and second reaction kettle is replenished by the 3rd reaction kettle, with the Na for preparing
2CO
3Solution replenishes in the 3rd reaction kettle; The SO that first reaction kettle fails to sponge
2, get into second and third reaction kettle through pipeline and carry out the absorption of two steps, absorb the tail gas of handling through three grades of alkali lye and enter the people absorption tower again through emptying after the alkali cleaning, final deflated purification rate is 99%.
(3) slurries that contain Sodium Pyrosulfite that step (2) made are centrifugal, obtain Sodium Pyrosulfite wet feed and liquid, and gained liquid is called mother liquor; Mother liquor continues on for Na
2CO
3The preparation of solution;
(4) the Sodium Pyrosulfite wet feed that step (3) is obtained obtains the Sodium Pyrosulfite finished product through super-dry, and purity is 95.3, to the requirement of technical grade Sodium Pyrosulfite.
Embodiment 2
(1) acyl chlorides is produced tail gas through washing, removes HCl gas wherein;
(2) acyl chlorides handled of step (1) is produced tail gas with 180g/L, 47 ℃ Na
2CO
3Solution carries out three grades of alkali lye and absorbs, and the acyl chlorides that step (1) was handled is produced tail gas and fed first reaction kettle and Na
2CO
3Solution reaction is along with SO
2Absorption, slurry color is pale yellow to deep yellow by leucismus, again by deep yellow shoal yellow in vain; When slurry color when white and pH value is 4.5 by xanthochromia, absorption reaction is reached home, and obtains containing the slurries of Sodium Pyrosulfite; From first reaction kettle, emit the slurries that contain Sodium Pyrosulfite; First reaction kettle reduces slurries and is replenished by second reaction kettle, and second reaction kettle is replenished by the 3rd reaction kettle, with the Na for preparing
2CO
3Solution replenishes in the 3rd reaction kettle; The SO that first reaction kettle fails to sponge
2, get into second and third reaction kettle through pipeline and carry out the absorption of two steps, absorb the tail gas of handling through three grades of alkali lye and enter the people absorption tower again through emptying after the alkali cleaning, final deflated purification rate is 99%.
(3) slurries that contain Sodium Pyrosulfite that step (2) made are centrifugal, obtain Sodium Pyrosulfite wet feed and liquid, and gained liquid is called mother liquor; Mother liquor continues on for Na
2CO
3The preparation of solution;
(4) the Sodium Pyrosulfite wet feed that step (3) is obtained obtains the Sodium Pyrosulfite finished product through super-dry, and purity is 95.7%, to the requirement of technical grade Sodium Pyrosulfite.
Embodiment 3
(1) acyl chlorides is produced tail gas through washing, removes HCl gas wherein;
(2) acyl chlorides handled of step (1) is produced tail gas with 160g/L, 45 ℃ Na
2CO
3Solution carries out three grades of alkali lye and absorbs, and the acyl chlorides that step (1) was handled is produced tail gas and fed first reaction kettle and Na
2CO
3Solution reaction is along with SO
2Absorption, slurry color is pale yellow to deep yellow by leucismus, again by deep yellow shoal yellow in vain; When slurry color when white and pH value is 4.0 by xanthochromia, absorption reaction is reached home, and obtains containing the slurries of Sodium Pyrosulfite; From first reaction kettle, emit the slurries that contain Sodium Pyrosulfite; First reaction kettle reduces slurries and is replenished by second reaction kettle, and second reaction kettle is replenished by the 3rd reaction kettle, with the Na for preparing
2CO
3Solution replenishes in the 3rd reaction kettle; The SO that first reaction kettle fails to sponge
2, get into second and third reaction kettle through pipeline and carry out the absorption of two steps, absorb the tail gas of handling through three grades of alkali lye and enter the people absorption tower again through emptying after the alkali cleaning, final deflated purification rate is 99%.
(3) slurries that contain Sodium Pyrosulfite that step (2) made are centrifugal, obtain Sodium Pyrosulfite wet feed and liquid, and gained liquid is called mother liquor; Mother liquor continues on for Na
2CO
3The preparation of solution;
(4) the Sodium Pyrosulfite wet feed that step (3) is obtained obtains the Sodium Pyrosulfite finished product through super-dry, and purity is 95.2%, to the requirement of technical grade Sodium Pyrosulfite.
Above-described embodiment describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the prerequisite of spirit not breaking away from the present invention; Various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (5)
1. one kind is utilized acyl chlorides to produce the method that tail gas prepares the technical grade Sodium Pyrosulfite, it is characterized in that: may further comprise the steps:
(1) acyl chlorides is produced tail gas through washing, removes HCl gas wherein;
(2) acyl chlorides handled of step (1) is produced tail gas and is used the Na of concentration as 150-180g/L
2CO
3Solution absorption SO
2, the acyl chlorides that step (1) was handled is produced tail gas and Na
2CO
3The liquid that solution reaction obtains is called slurries, and when slurry color when white and pH value is 3.5-4.5 by xanthochromia, absorption reaction is reached home, and obtains containing the slurries of Sodium Pyrosulfite;
(3) slurries that contain Sodium Pyrosulfite that step (2) made are centrifugal, obtain Sodium Pyrosulfite wet feed and liquid, and gained liquid is called mother liquor;
(4) the Sodium Pyrosulfite wet feed that step (3) is obtained obtains the Sodium Pyrosulfite finished product through super-dry.
2. the acyl chlorides that utilizes according to claim 1 is produced the method that tail gas prepares the technical grade Sodium Pyrosulfite, it is characterized in that: said Na
2CO
3The temperature of solution is 43-47 ℃.
3. the acyl chlorides that utilizes according to claim 2 is produced the method that tail gas prepares the technical grade Sodium Pyrosulfite, and wherein white and pH value is 4.0 o'clock to slurry color described in the step (2) by xanthochromia, and absorption reaction is reached home.
4. the acyl chlorides that utilizes according to claim 3 is produced the method that tail gas prepares the technical grade Sodium Pyrosulfite, and it is characterized in that: the acyl chlorides that said step (1) was handled is produced tail gas and used Na
2CO
3It is to adopt three grades of alkali lye to absorb that solution absorbs.
5. the acyl chlorides that utilizes according to claim 4 is produced the method that tail gas prepares the technical grade Sodium Pyrosulfite, and it is characterized in that: wherein mother liquor is used for preparing once more Na described in the step (3)
2CO
3Solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104063364A CN102515209A (en) | 2011-12-08 | 2011-12-08 | Method for preparing industrial-grade sodium pyrosulfite from tail gas generated in production of acyl chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104063364A CN102515209A (en) | 2011-12-08 | 2011-12-08 | Method for preparing industrial-grade sodium pyrosulfite from tail gas generated in production of acyl chloride |
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| Publication Number | Publication Date |
|---|---|
| CN102515209A true CN102515209A (en) | 2012-06-27 |
Family
ID=46286361
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104063364A Pending CN102515209A (en) | 2011-12-08 | 2011-12-08 | Method for preparing industrial-grade sodium pyrosulfite from tail gas generated in production of acyl chloride |
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|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104150512A (en) * | 2014-08-13 | 2014-11-19 | 梅州联进化工有限公司 | Production process of sodium pyrosulfite |
| CN104386714A (en) * | 2014-11-13 | 2015-03-04 | 武穴市融锦化工有限公司 | Preparation method of food-grade sodium pyrosulfite |
| CN110743344A (en) * | 2019-10-10 | 2020-02-04 | 株洲三特环保节能股份有限公司 | Method for removing low-concentration sulfur dioxide in flue gas and preparing sodium metabisulfite |
| CN112250089A (en) * | 2020-10-29 | 2021-01-22 | 新晃鲁湘钡业有限公司 | Method for producing sodium metabisulfite by utilizing sulfur-containing tail gas |
Citations (4)
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|---|---|---|---|---|
| US3860695A (en) * | 1972-04-29 | 1975-01-14 | Hoechst Ag | Process for the manufacture of sodium pyrosulfite |
| US3995015A (en) * | 1975-03-27 | 1976-11-30 | Allied Chemical Corporation | Process for making sodium metabisulfite |
| US4127642A (en) * | 1976-06-24 | 1978-11-28 | Virginia Chemicals Inc. | Production of sodium dithionite from sulfur dioxide, sodium formate, and sodium carbonate with minimum quantities of water and methanol |
| US5976485A (en) * | 1996-10-07 | 1999-11-02 | Solvay Minerals, Inc. | Sodium metabisulfite process |
-
2011
- 2011-12-08 CN CN2011104063364A patent/CN102515209A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| US3860695A (en) * | 1972-04-29 | 1975-01-14 | Hoechst Ag | Process for the manufacture of sodium pyrosulfite |
| US3995015A (en) * | 1975-03-27 | 1976-11-30 | Allied Chemical Corporation | Process for making sodium metabisulfite |
| US4127642A (en) * | 1976-06-24 | 1978-11-28 | Virginia Chemicals Inc. | Production of sodium dithionite from sulfur dioxide, sodium formate, and sodium carbonate with minimum quantities of water and methanol |
| US5976485A (en) * | 1996-10-07 | 1999-11-02 | Solvay Minerals, Inc. | Sodium metabisulfite process |
Non-Patent Citations (2)
| Title |
|---|
| 孙轶: "焦亚硫酸钠及其生产工艺", 《化工生产与技术》 * |
| 徐耀荣: "利用焙烧硫化锌矿炉气中SO2生产焦亚硫酸钠", 《无机盐工业》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104150512A (en) * | 2014-08-13 | 2014-11-19 | 梅州联进化工有限公司 | Production process of sodium pyrosulfite |
| CN104386714A (en) * | 2014-11-13 | 2015-03-04 | 武穴市融锦化工有限公司 | Preparation method of food-grade sodium pyrosulfite |
| CN104386714B (en) * | 2014-11-13 | 2016-09-07 | 武穴市融锦化工有限公司 | The method of preparation food-grade sodium pyrosulfite |
| CN110743344A (en) * | 2019-10-10 | 2020-02-04 | 株洲三特环保节能股份有限公司 | Method for removing low-concentration sulfur dioxide in flue gas and preparing sodium metabisulfite |
| CN110743344B (en) * | 2019-10-10 | 2021-12-14 | 株洲湘三特环保有限公司 | Method for removing low-concentration sulfur dioxide in flue gas and preparing sodium metabisulfite |
| CN112250089A (en) * | 2020-10-29 | 2021-01-22 | 新晃鲁湘钡业有限公司 | Method for producing sodium metabisulfite by utilizing sulfur-containing tail gas |
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Application publication date: 20120627 |