CN101343038A - Recovery method for mix waste gas of hydrogen chloride and sulphur dioxide in lipoic acid preparation - Google Patents
Recovery method for mix waste gas of hydrogen chloride and sulphur dioxide in lipoic acid preparation Download PDFInfo
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- CN101343038A CN101343038A CNA2008100222590A CN200810022259A CN101343038A CN 101343038 A CN101343038 A CN 101343038A CN A2008100222590 A CNA2008100222590 A CN A2008100222590A CN 200810022259 A CN200810022259 A CN 200810022259A CN 101343038 A CN101343038 A CN 101343038A
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Abstract
Disclosed is a recovering method for the mixture waste gas of the chlorine hydride and the sulfur dioxide in the thioctic acid production, which belongs to the mixture waste gas recovery technical field in the thioctic acid production. The recovering method includes that the mixture waste gas of the chlorine hydride and the sulfur dioxide is introduced to a water absorption device through the pipeline; when the concentration of the chlorine hydride solution in the water absorption reaches the discharge concentration, the chlorine hydride is recovered; the purified sulfur dioxide gas after the adsorption of the chlorine hydride gas is sucked to the reactor device by the pipeline in the vacuum way and reacts with the sodium hydroxide solution in steps while the chlorine hydride gas is absorbed by the water absorption device; the reaction temperature and the PH value are respectively controlled and adjusted in steps so that the sodium sulfite solution is obtained; the sodium sulfite solution is discharged from the reactor device and fed to a centrifugal separation device for centrifugal separation, so as to obtain the seven hydrate sodium sulfite crystal; the mother liquor obtained through the centrifugal separation is fed to the reactor device again. The recovering method for the mixture waste gas of the chlorine hydride and the sulfur dioxide has the advantages of environmental protection, resource maximum utilization and saving production cost for the thioctic acid production enterprises.
Description
Technical field
The invention belongs to the recovery technology field of the mix waste gas of Thioctic Acid in producing, be specifically related to a kind of Thioctic Acid in producing hydrogenchloride and the recovery method of sulfurous gas mix waste gas.
Background technology
As the industry's knowledge of the reason, need to use the sulfur oxychloride chlorination reaction in the chloride process of Thioctic Acid intermediate monoethyl adipatee and 6-hydroxyl-8-chloroctanoic acid ethyl ester, can produce a large amount of hydrogenchloride and the useless body of sulfurous gas mixing in reaction process, reaction equation is as follows:
In the prior art, normally hydrogenchloride and sulfurous gas mix waste gas are directly discharged to the external world, thereby cause following problem: at first, this mix waste gas is directly arranged to the external world, caused severe contamination environment; Secondly, can cause the unreasonable waste of resource, because hydrochloric acid and S-WAT are widely used in the production of Chemicals, and S-WAT consumes the environmentfriendly products of sulfurous gas and has vast market prospect as a kind of; Also have, cause the increase of Thioctic Acid manufacturing enterprise self cost because the hydrolysis of the preparation of monoethyl adipatee in the production of Thioctic Acid, Thioctic Acid ethyl ester in and operation need use a large amount of hydrogenchloride, can save the production cost of Thioctic Acid.
In view of this,, have very positive meaning so undoubtedly, that is: help the environment of protecting the mankind to depend on for existence if the mix waste gas of hydrogenchloride in the Thioctic Acid production and sulfurous gas can be reclaimed; Help making full use of of resource; Help enterprise self and save cost.The applicant retrieves, and does not search the technology enlightenment with hydrogenchloride and the comprehensive utilization of sulfurous gas mix waste gas in existing literature, and in the industry cycle (Thioctic Acid production industry) do not hear the report that success is arranged yet.The technical scheme that the present invention will introduce below is based on producing under this background.
Summary of the invention
Task of the present invention be to provide a kind of Thioctic Acid that helps protecting environment, economize on resources and reduce the production cost of enterprise self in producing hydrogenchloride and the recovery method of sulfurous gas mix waste gas.
Task of the present invention is finished like this, the hydrogenchloride during a kind of Thioctic Acid is produced and the recovery method of sulfurous gas mix waste gas, it is that hydrogenchloride and sulfurous gas mix waste gas are incorporated into by more than at least one cover and the water absorption unit that the confession hydrogen chloride gas is dissolved in the water that is used for that be one another in series and connect by pipeline, when reaching blowing concentration, the concentration of the hydrogen chloride solution in the water absorption unit reclaims hydrogenchloride, the sulfur dioxide gas vacuum of the purification that is obtained after with the absorbing hydrogen chloride gas in the water absorption unit by pipeline in by water absorption unit absorbing hydrogen chloride gas is drawn in the reaction unit and the sodium hydroxide solution stepwise reaction, and substep control reaction temperature and adjusted stepwise pH value, obtain sodium sulfite solution, sodium sulfite solution is discharged to centrifugation the centrifugal separating device from reaction unit, obtain seven water S-WAT xln, the mother liquor that centrifugation goes out is sent back in the reaction unit.
In a specific embodiment of the present invention, the quantity of described water absorption unit is five covers.
In another specific embodiment of the present invention, the quantity of described water absorption unit is three covers.
In also specific embodiment of the present invention, described water absorption unit comprises that absorption tower and being used to of being connected with the absorption tower hold the storage tank of the water that absorbing hydrogen chloride gas uses.
In another specific embodiment of the present invention, described water is any one in tap water, river, deionized water, underground water or the phreatic water.
In another specific embodiment of the present invention, described water is tap water.
More of the present invention and in specific embodiment, described reaction unit is to have the reactor of water towards pump; Described centrifugal separating device is a whizzer.
In of the present invention and then specific embodiment, described blowing concentration be meant the degree of depth of hydrogen chloride solution reach 〉=30%.
Of the present invention again more and in specific embodiment, described stepwise reaction, substep control reaction temperature and adjusted stepwise pH value are meant, earlier vacuum is drawn into sulfur dioxide gas and sodium hydroxide solution contact reacts in the reaction unit, control reaction temperature is 40～60 ℃, regulate pH value to 5.0～6.5, obtain reaction soln, and then reaction soln is transferred to adds sodium hydroxide solution in another reaction unit and in reaction soln, control reaction temperature is 40～60 ℃, and the pH value of conditioned reaction solution is 9.0～10.0.
In again of the present invention and then specific embodiment, the concentration of described sodium hydroxide solution is 10～50%.
The advantage of the technical scheme that the present invention recommended: can reclaim hydrogen chloride solution and seven water S-WATs respectively with directly draining into extraneous hydrogenchloride and sulfurous gas mix waste gas in the prior art; both helped the guard ring border; help the resource maximum using again; also can be Thioctic Acid manufacturing enterprise saves production cost; because the hydrogen chloride solution that reclaims can be incorporated in the production process of Thioctic Acid, but and seven water S-WAT supply markets are used to produce S-WAT series products such as sodium sulphite anhydrous 99.3.
Description of drawings
Accompanying drawing be the employed water absorption unit of the inventive method and with the synoptic diagram of the reaction unit of water absorption unit pipeline connection.
Embodiment
Embodiment 1:
Ask for an interview accompanying drawing; hydrogenchloride and sulfurous gas mix waste gas that the sulfur oxychloride chlorination reaction that acidylate liquid in Thioctic Acid intermediate reduced liquid and the chloride process is adopted by pipeline 1 is produced are incorporated in the water absorption unit 2; in the present embodiment, the applicant has selected for use three to overlap the water absorption unit 2 that the confession hydrogen chloride gas is dissolved in the water that is used for that is one another in series and connects.According to the technology general knowledge that industry is familiar with, hydrogen chloride gas is soluble in water, and sulfurous gas is insoluble in water, and the applicant is just according to implementing to reclaim in this reason.Every cover water absorption unit 2 comprises absorption tower 21 and passes through first, second pipeline 221,222 storage tanks 22 that are connected with absorption tower 21 pipelines, after hydrogenchloride and sulfurous gas mix waste gas enter the absorption tower 21 of a cover absorption unit 2 that first cover is the illustrated left side, enter into storage tank 22 by first pipeline 221, constitute pump around circuit by the effect that is located at the recycle pump 223 on second pipeline 222, hydrogen chloride gas in hydrogenchloride and the sulfurous gas mix waste gas is dissolved in the storage tank 22 that fills tap water fully, the blowing concentration of the hydrogen chloride solution in storage tank 22 through sampling and measuring reach 〉=30%, emit and promptly reclaim hydrogen chloride solution.Before blowing, close first valve 2221 and first valve 2221 of closing on second pipeline 222 that is located at the 3rd cover water absorption unit 2 on second pipeline 222 that is located at the second cover water absorption unit 2, open second valve 2251 on the 4th pipeline 225, under the work of the recycle pump separately 223 of three cover water absorption units 2, making hydrogen chloride solution in the storage tank 22 of second cover and the 3rd cover water absorption unit 2 be transferred to first cover is in the storage tank 22 on the left side shown in the drawings.Owing to there are three storage tanks 22, therefore to the end not a storage tank 22 blow-off valve on each storage tank 22 226 should be opened when promptly a storage tank 22 on the right is mended entry (tap water), after moisturizing finishes, closed again.After the first cover water absorption unit 2 reclaims hydrogenchloride, continuation is through second, the 3rd cover is centre shown in the drawings one cover and the right one cover water absorption unit, 2 absorbing hydrogen chloride gases, detailed process is with the first cover water absorption unit 2, respectively pass through the 3rd pipeline 224 connect in series between the first cover water absorption unit 2 and the second cover water absorption unit 2 and the second cover water absorption unit 2 and the 3rd cover water absorption unit 2, and between three storage tanks 22 also by the 4th pipeline 225 connect in series that are equipped with second valve 2251, hydrogen chloride gas in the mix waste gas fully can be absorbed through three cover water absorption units 2, be that sulfur dioxide gas vacuum that the 3rd pipeline 224 of storage tank 22 of water absorption unit 2 of illustrated the right one cover has obtained purifying after with the intact hydrogen chloride gas of absorption in the three cover water absorption units 2 sucks or claims negative pressure to be drawn in the reaction unit and the sodium hydroxide solution stepwise reaction by last cover in the time of again by three cover water absorption units, 2 absorbing hydrogen chloride gases, and substep control reaction temperature and adjusted stepwise pH value.Specifically: reaction unit is to have the reactor 3 of water towards pump 31, will enter into the sulfur dioxide gas of reactor 3 and 32% sodium hydroxide solution reaction, and 50 ℃ of control reaction temperature are regulated pH value to 5.6, obtain reaction soln; Again reaction soln is switched to and continue in another reactor that does not provide in the drawings and the sodium hydroxide solution reaction, promptly continue to absorb sulfur dioxide gas, it specifically is the sodium hydroxide solution of adding 32% in this reactor, control reaction temperature is 50 ℃, until the pH value is adjusted to pH9.5 by previous 5.6, obtain sodium sulfite solution, and regulating water coolant is the flow of icy salt solution, under whipped state, make the sodium sulfite solution cooling, when reaching 30 ℃, temperature separates out the xln of seven a large amount of aqueous sodium persulfates, when temperature reaches 20 ℃, the whizzer that material is put into as centrifugal device from reactor separates drying, obtain seven water S-WAT xln finished products, the isolated mother liquor of whizzer enters the mother liquor pond and applied mechanically by pumped back reactor 3 joins alkali, the content of resulting seven water S-WATs is 48.5%, meets the requirement of national standard first grade.The reaction formula that present embodiment reclaims sulfur dioxide gas is:
2NaOH+SO
2＝Na
2SO
4+H
2O
Na
2SO
4+H
2O+SO
2＝2NaHSO
3
NaHSO
3+NaOH＝Na
2SO
4+H
2O
Na
3SO
4·7H
2O＝Na
3SO
47H
2O。
Embodiment 2:
Control stepwise reaction condition: naoh concentration is 10%, and temperature of reaction is 40 ℃, regulates pH to 5.0; In another reactor, naoh concentration is 10%, and temperature of reaction is 40 ℃, adjusts pH to 9.0, and the content of resulting seven water S-WATs is 48.7%, meets the requirement of national standard first grade, and all the other are all with the description to embodiment 1.
Embodiment 3:
Control stepwise reaction condition: naoh concentration is 10%, and temperature of reaction is 50 ℃, regulates pH to 6.0; Switch to another reactor from reactor 3 at reaction solution, naoh concentration is 10%, and temperature of reaction is 50 ℃, adjust pH to 9.5, the content of resulting seven water S-WATs is 48.3%, meets the requirement of national standard first grade, and all the other are all with the description to embodiment 1.
Embodiment 4:
Control stepwise reaction condition: naoh concentration is 50%, and temperature of reaction is 60 ℃, regulates pH to 6.5; Switch to another reactor from reactor 3 at reaction solution, naoh concentration is 50%, and temperature of reaction is 60 ℃, adjust pH to 10.0, the content of resulting seven water S-WATs is 48.1%, meets the requirement of national standard first grade, and all the other are all with the description to embodiment 1.
Embodiment 5:
Control stepwise reaction condition: naoh concentration is 50%, and temperature of reaction is 40 ℃, regulates pH to 5.5; Switch to another reactor from reactor 3 at reaction solution, naoh concentration is 50%, and temperature of reaction is 40 ℃, adjust pH to 10.0, the content of resulting seven water S-WATs is 48.8%, meets the requirement of national standard first grade, and all the other are all with the description to embodiment 1.
Embodiment 6:
Control stepwise reaction condition: naoh concentration is 30%, and temperature of reaction is 60 ℃, regulates pH to 5.5; Switch to another reactor from reactor 3 at reaction solution, naoh concentration is 30%, and temperature of reaction is 60 ℃, adjust pH to 10.0, the content of resulting seven water S-WATs is 48.3%, meets the requirement of national standard first grade, and all the other are all with the description to embodiment 1.
Embodiment 7:
Control stepwise reaction condition: naoh concentration is 30%, and temperature of reaction is 50 ℃, regulates pH to 6.0; Switch to another reactor from reactor 3 at reaction solution, naoh concentration is 30%, and temperature of reaction is 50 ℃, adjust pH to 9.5, the content of resulting seven water S-WATs is 48.4%, meets the requirement of national standard first grade, and all the other are all with the description to embodiment 1.
Embodiment 8:
Control stepwise reaction condition: naoh concentration is 50%, and temperature of reaction is 50 ℃, regulates pH to 6.0; Switch to another reactor from reactor 3 at reaction solution, naoh concentration is 50%, and temperature of reaction is 50 ℃, adjust pH to 9.5, the content of resulting seven water S-WATs is 48.2%, meets the requirement of national standard first grade, and all the other are all with the description to embodiment 1.
Claims (10)
1, the hydrogenchloride during a kind of Thioctic Acid is produced and the recovery method of sulfurous gas mix waste gas, it is characterized in that it is that hydrogenchloride and sulfurous gas mix waste gas are incorporated into by more than at least one cover and the water absorption unit that the confession hydrogen chloride gas is dissolved in the water that is used for that be one another in series and connect by pipeline, when reaching blowing concentration, the concentration of the hydrogen chloride solution in the water absorption unit reclaims hydrogenchloride, the sulfur dioxide gas vacuum of the purification that is obtained after with the absorbing hydrogen chloride gas in the water absorption unit by pipeline in by water absorption unit absorbing hydrogen chloride gas is drawn in the reaction unit and the sodium hydroxide solution stepwise reaction, and substep control reaction temperature and adjusted stepwise pH value, obtain sodium sulfite solution, sodium sulfite solution is discharged to centrifugation the centrifugal separating device from reaction unit, obtain seven water S-WAT xln, the mother liquor that centrifugation goes out is sent back in the reaction unit.
2, the hydrogenchloride during Thioctic Acid according to claim 1 is produced and the recovery method of sulfurous gas mix waste gas, the quantity that it is characterized in that described water absorption unit is five covers.
3, the hydrogenchloride during Thioctic Acid according to claim 1 is produced and the recovery method of sulfurous gas mix waste gas, the quantity that it is characterized in that described water absorption unit is three covers.
4, the hydrogenchloride in producing according to claim 1 or 2 or 3 described Thioctic Acids and the recovery method of sulfurous gas mix waste gas is characterized in that described water absorption unit comprises that absorption tower and being used to of being connected with the absorption tower hold the storage tank of the water that absorbing hydrogen chloride gas uses.
5, the hydrogenchloride during Thioctic Acid according to claim 4 is produced and the recovery method of sulfurous gas mix waste gas is characterized in that described water is any one in tap water, river, deionized water, underground water or the phreatic water.
6, the hydrogenchloride during Thioctic Acid according to claim 5 is produced and the recovery method of sulfurous gas mix waste gas is characterized in that described water is tap water.
7, the hydrogenchloride during Thioctic Acid according to claim 1 is produced and the recovery method of sulfurous gas mix waste gas is characterized in that described reaction unit is to have the reactor of water towards pump; Described centrifugal separating device is a whizzer.
8, the hydrogenchloride during Thioctic Acid according to claim 1 is produced and the recovery method of sulfurous gas mix waste gas, it is characterized in that described blowing concentration be meant the degree of depth of hydrogen chloride solution reach 〉=30%.
9, the hydrogenchloride during Thioctic Acid according to claim 1 is produced and the recovery method of sulfurous gas mix waste gas, it is characterized in that described stepwise reaction, substep control reaction temperature and adjusted stepwise pH value are meant, earlier vacuum is drawn into sulfur dioxide gas and sodium hydroxide solution contact reacts in the reaction unit, control reaction temperature is 40～60 ℃, regulate pH value to 5.0～6.5, obtain reaction soln, and then reaction soln is transferred to adds sodium hydroxide solution in another reaction unit and in reaction soln, control reaction temperature is 40～60 ℃, and the pH value of conditioned reaction solution is 9.0～10.0.
10, according to the hydrogenchloride in claim 1 or the 9 described Thioctic Acids productions and the recovery method of sulfurous gas mix waste gas, the concentration that it is characterized in that described sodium hydroxide solution is 10～50%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100222590A CN101343038A (en) | 2008-06-30 | 2008-06-30 | Recovery method for mix waste gas of hydrogen chloride and sulphur dioxide in lipoic acid preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100222590A CN101343038A (en) | 2008-06-30 | 2008-06-30 | Recovery method for mix waste gas of hydrogen chloride and sulphur dioxide in lipoic acid preparation |
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|---|---|
| CN101343038A true CN101343038A (en) | 2009-01-14 |
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| CNA2008100222590A Pending CN101343038A (en) | 2008-06-30 | 2008-06-30 | Recovery method for mix waste gas of hydrogen chloride and sulphur dioxide in lipoic acid preparation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102343197A (en) * | 2011-10-18 | 2012-02-08 | 褚平忠 | Method for separating and recovering mixed gas of hydrogen chloride and sulfur dioxide |
| CN102512931A (en) * | 2011-12-08 | 2012-06-27 | 烟台泰和新材料股份有限公司 | Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production |
| CN107899403A (en) * | 2017-11-30 | 2018-04-13 | 成武县晨晖环保科技有限公司 | Chloroethene acylating acid method produces the tail gas sulphur dioxide sulfur method of chloracetyl chloride |
| CN109970082A (en) * | 2019-05-06 | 2019-07-05 | 黄石加柯环保科技有限公司 | A method of high-pure anhydrous sodium sulfite is prepared using relieving haperacidity flue gas |
-
2008
- 2008-06-30 CN CNA2008100222590A patent/CN101343038A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102343197A (en) * | 2011-10-18 | 2012-02-08 | 褚平忠 | Method for separating and recovering mixed gas of hydrogen chloride and sulfur dioxide |
| CN102512931A (en) * | 2011-12-08 | 2012-06-27 | 烟台泰和新材料股份有限公司 | Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production |
| CN102512931B (en) * | 2011-12-08 | 2014-04-16 | 烟台泰和新材料股份有限公司 | Method for preparing sodium hydrosulphite by utilization of tail gas from acyl chloride production |
| CN107899403A (en) * | 2017-11-30 | 2018-04-13 | 成武县晨晖环保科技有限公司 | Chloroethene acylating acid method produces the tail gas sulphur dioxide sulfur method of chloracetyl chloride |
| CN109970082A (en) * | 2019-05-06 | 2019-07-05 | 黄石加柯环保科技有限公司 | A method of high-pure anhydrous sodium sulfite is prepared using relieving haperacidity flue gas |
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Open date: 20090114 |