CN104707464A - HCl gas recovery method under high vacuum condition - Google Patents
HCl gas recovery method under high vacuum condition Download PDFInfo
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- CN104707464A CN104707464A CN201510113466.7A CN201510113466A CN104707464A CN 104707464 A CN104707464 A CN 104707464A CN 201510113466 A CN201510113466 A CN 201510113466A CN 104707464 A CN104707464 A CN 104707464A
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Abstract
The invention discloses an HCl gas recovery method under a high vacuum condition. The HCl gas recovery method comprises the following steps: interconnecting five-stage absorption systems, wherein a concentrated hydrochloric acid system is used as the first stage, a diluted hydrochloric acid is used as the second stage, a weak hydrochloric acid is used as the third stage, a washing system is used as the fourth stage, and an alkaline wash system is used as the fifth stage; continuously carrying out five-stage forced circulation and cooling packed tower adsorption to the HCl gas at an absolute pressure lower than 1,500 Pa and under am ambient temperature condition. The HCl gas recovery method disclosed by the invention has the following advantages: firstly, the absorption efficiency of the HCl gas at the absolution pressure less than 1,500 Pa is up to 99.5%; secondly, the HCl gas recovery method is continuous in operation, simple and reliable in process, convenient to operate and high in safety; thirdly, the HCl gas recovery method improves the high vacuum possibility for production of phosphite ester and phosphate, and increases the yield of the production of phosphite ester and phosphate; fourthly, the method greatly reduces gas emission and wastewater discharge.
Description
Technical field
The present invention relates to a kind of HCl Gas recovery method under serialization high vacuum condition, especially relate to the HC1 Gas recovering method under a kind of high vacuum condition.
Background technology
Hydrogen chloride, a hydrogen chloride molecule is made up of a chlorine atom and a hydrogen atom.Molecular formula is HCl.The aqueous solution is commonly called as hydrochloric acid, formal name used at school hydrochloric acid.Hydrogen chloride is the gas of colourless and irritant smell, and hydrogen chloride is soluble in water, and 0 DEG C time, the water of 1 volume approximately can dissolve the hydrogen chloride of 500 volumes; Hydrogen chloride is mainly used in system dye, spices, medicine, various chloride and corrosion inhibitor, and relative molecular mass is 36.5.
In Chemical Manufacture, have much chemical reaction by-product HCl gas, recycle fairly perfect, ripe at condition of normal pressure HCl, the rate of recovery and by-product hydrochloric acid concentration can meet production requirement.But it is large to reclaim HCl gas difficulty under vacuum, and particularly vacuum is high, and absolute pressure is low at the recovery utilization rate of below 1500Pa HCl gas, and by-product hydrochloric acid concentration does not reach 31%, toxic emission and neutralized wastewater amount large.
Summary of the invention
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A HCl Gas recovering method under high vacuum condition, comprises Pyatyi absorption system and is interconnected:
(1) first order is concentrated hydrochloric acid system, and concentrated hydrochloric acid tower cyclic absorption HCl gas concentration is 28 ~ 32%, preferably 31%, and temperature 10 ~ 20 DEG C, preferably 15 DEG C, internal circulating load 3 ~ 15m3/h, preferred 10m3/h; Concentrated hydrochloric acid adopts continuous feeding and discharging mode, and by second level watery hydrochloric acid groove continuous supplementation to concentrated hydrochloric acid groove, 31% concentrated hydrochloric acid exports from concentrated hydrochloric acid pump continuously; Packed tower diameter is determined according to HCl treating capacity, and HCl gas flow velocity in tower is 0.2 ~ 1.0m/s, preferred 0.5m/s.
(2) second level is watery hydrochloric acid system watery hydrochloric acid tower circulation watery hydrochloric acid concentration is 15 ~ 20%, preferably 18%, and temperature 10 ~ 20 DEG C, preferably 15 DEG C, internal circulating load 3 ~ 15m3/h, preferred 10m3/h; Watery hydrochloric acid adopts continuous feeding and discharging mode, and the watery hydrochloric acid groove of watery hydrochloric acid absorption system flows into concentrated hydrochloric acid groove by liquid level difference continuously.
(3) third level is weak hydrochloric acid system, and weak hydrochloric acid groove utilizes liquid level difference to continuously flow into watery hydrochloric acid groove, and the weak hydrochloric acid tower cyclic absorption concentration of weak hydrochloric acid absorption system is 5 ~ 10%, preferably 8%, and temperature 10 ~ 20 DEG C, preferably 15 DEG C, internal circulating load 3 ~ 15m3/h, preferred 10m3/h; Weak hydrochloric acid adopts continuous feeding and discharging mode, and the weak hydrochloric acid groove of weak hydrochloric acid absorption system flows into watery hydrochloric acid groove by liquid level difference continuously.
(4) fourth stage is water wash system, and water scrubber circulating absorption solution is 1 ~ 5% containing HCl concentration, preferably 2%, absorb temperature 10 ~ 20 DEG C, preferably 15 DEG C, internal circulating load 3 ~ 15m3/h, preferred 10m3/h; Water wash system adopts continuous running water to add to rinsing bowl, and keeps the liquid level of rinsing bowl, and water magnitude of recruitment is determined by HCl is gas generated.
(5) level V is caustic washing system, and lye tank (vat) abNaOH concentration is 2 ~ 5%, preferably 3%, and alkali cleaning internal circulating load 3 ~ 15m3/h, preferred 10m3/h, alkali cleaning temperature 10 ~ 20 DEG C, preferably 15 DEG C; Lye tank (vat) has two can carry out handover operation, will switch when alkali wash water reaches pH8, prevents HCl gas from entering vacuum suction unit, causes unit acidity to destroy.
Advantage of the present invention is that the absorption efficiency of the first, HCl gas under absolute pressure < 1500Pa condition can reach 99.5%; The second, serialization operation, simple and reliable process, easy to operate, security is high; 3rd, the present invention is that phosphite ester and phosphate produce the possibility improving high vacuum, improves the yield of phosphite ester and phosphate production; 4th, the present invention greatly reduces gas discharging and wastewater discharge.
Detailed description of the invention
A HCl Gas recovering method under high vacuum condition, comprises Pyatyi absorption system and is interconnected:
(1) first order is concentrated hydrochloric acid system, and concentrated hydrochloric acid tower cyclic absorption HCl gas concentration is 28 ~ 32%, preferably 31%, and temperature 10 ~ 20 DEG C, preferably 15 DEG C, internal circulating load 3 ~ 15m3/h, preferred 10m3/h; Concentrated hydrochloric acid adopts continuous feeding and discharging mode, and by second level watery hydrochloric acid groove continuous supplementation to concentrated hydrochloric acid groove, 31% concentrated hydrochloric acid exports from concentrated hydrochloric acid pump continuously; Packed tower diameter is determined according to HCl treating capacity, and HCl gas flow velocity in tower is 0.2 ~ 1.0m/s, preferred 0.5m/s.
(2) second level is watery hydrochloric acid system watery hydrochloric acid tower circulation watery hydrochloric acid concentration is 15 ~ 20%, preferably 18%, and temperature 10 ~ 20 DEG C, preferably 15 DEG C, internal circulating load 3 ~ 15m3/h, preferred 10m3/h; Watery hydrochloric acid adopts continuous feeding and discharging mode, and the watery hydrochloric acid groove of watery hydrochloric acid absorption system flows into concentrated hydrochloric acid groove by liquid level difference continuously.
(3) third level is weak hydrochloric acid system, and weak hydrochloric acid groove utilizes liquid level difference to continuously flow into watery hydrochloric acid groove, and the weak hydrochloric acid tower cyclic absorption concentration of weak hydrochloric acid absorption system is 5 ~ 10%, preferably 8%, and temperature 10 ~ 20 DEG C, preferably 15 DEG C, internal circulating load 3 ~ 15m3/h, preferred 10m3/h; Weak hydrochloric acid adopts continuous feeding and discharging mode, and the weak hydrochloric acid groove of weak hydrochloric acid absorption system flows into watery hydrochloric acid groove by liquid level difference continuously.
(4) fourth stage is water wash system, and water scrubber circulating absorption solution is 1 ~ 5% containing HCl concentration, preferably 2%, absorb temperature 10 ~ 20 DEG C, preferably 15 DEG C, internal circulating load 3 ~ 15m3/h, preferred 10m3/h; Water wash system adopts continuous running water to add to rinsing bowl, and keeps the liquid level of rinsing bowl, and water magnitude of recruitment is determined by HCl is gas generated.
(5) level V is caustic washing system, and lye tank (vat) abNaOH concentration is 2 ~ 5%, preferably 3%, and alkali cleaning internal circulating load 3 ~ 15m3/h, preferred 10m3/h, alkali cleaning temperature 10 ~ 20 DEG C, preferably 15 DEG C; Lye tank (vat) has two can carry out handover operation, will switch when alkali wash water reaches pH8, prevents HCl gas from entering vacuum suction unit, causes unit acidity to destroy.
Wherein, the specification of concentrated acid tower and watery hydrochloric acid tower or model are Φ=700mm, packed height 4m; The specification of weak hydrochloric acid tower, water scrubber, caustic wash tower or model are Φ=600mm, packed height 4m; The specification of cooler or model are graphite nahlock pass, F=15m2; Circulation pump size or model are Q=6.3m3/h, H=32m; The specification of circulating slot or model are V=5m3; The specification of lye tank (vat) or model are V=10m3.
Embodiment one: produce the HCl gas recycling and processing device under 5000t dimethylphosphite high vacuum condition per year.
First at the water of concentrated hydrochloric acid groove, watery hydrochloric acid groove, weak hydrochloric acid groove, rinsing bowl input 4m3, the 3%NaOH alkali lye of each 4m3 is configured at lye tank (vat) ab.
Pyatyi circulation absorption system carried out forced circulation and cools, making system keep running status.Open vacuum pump set, when system vacuum reaches below absolute pressure 1500Pa, dimethylphosphite production process normally starts to feed intake, along with the recovery of HCl gas, extraction concentrated hydrochloric acid can be exported from Countermeasure of Concentrated Acid Pump when by-product hydrochloric acid concentration reaches more than 31% in concentrated hydrochloric acid groove, concentrated hydrochloric acid produced quantity and phosphorus trichloride inventory match, and ratio is phosphorus trichloride: 31% hydrochloric acid=1:1.71; Add water in rinsing bowl, amount of water and POCl3 inventory ratio are phosphorus trichloride: water=1:1.18 simultaneously.
System is normally run rear 100t by-product hydrochloric acid consumption 3%NaOH alkali lye and is about 0.5m3, and the 3%NaOH alkali wash water of 4m3 can be guaranteed to reclaim by-product hydrochloric acid about 800t, when alkali wash water pH value reaches 8, need switch lye tank (vat) and ensure vacuum machine assembly air-exhausting not containing HCl gas.
Embodiment two: produce the HCl gas recycling and processing device under 5000t triethyl phosphate high vacuum condition per year.
First at the water of concentrated hydrochloric acid groove, watery hydrochloric acid groove, weak hydrochloric acid groove, rinsing bowl input 4m3, the 3%NaOH alkali lye of each 4m3 is configured at lye tank (vat) ab.
Pyatyi circulation absorption system carried out forced circulation and cools, making system keep running status.Open vacuum pump set, when system vacuum reaches below absolute pressure 1500Pa, triethyl phosphate production process normally starts to feed intake, along with the recovery of HCl gas, extraction concentrated hydrochloric acid can be exported from Countermeasure of Concentrated Acid Pump when by-product hydrochloric acid concentration reaches more than 31% in concentrated hydrochloric acid groove, concentrated hydrochloric acid produced quantity and POCl3 inventory match, and ratio is POCl3: 31% hydrochloric acid=1:2.30.Add water in rinsing bowl, amount of water and POCl3 inventory ratio are POCl3: water=1:1.587 simultaneously.
System is normally run rear 100t by-product hydrochloric acid consumption 3%NaOH alkali lye and is about 0.5m3, and the 3%NaOH alkali wash water of 4m3 can be guaranteed to reclaim by-product hydrochloric acid about 800t, when alkali wash water pH value reaches 8, need switch lye tank (vat) and ensure vacuum machine assembly air-exhausting not containing HCl gas.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (10)
1. the HCl Gas recovering method under high vacuum condition, comprises Pyatyi absorption system and is interconnected:
(1) first order is concentrated hydrochloric acid system, and concentrated hydrochloric acid tower cyclic absorption HCl gas concentration is 28 ~ 32%, temperature 10 ~ 20 DEG C, internal circulating load 3 ~ 15m3/h; Concentrated hydrochloric acid adopts continuous feeding and discharging mode, and by second level watery hydrochloric acid groove continuous supplementation to concentrated hydrochloric acid groove, 31% concentrated hydrochloric acid exports from concentrated hydrochloric acid pump continuously; Packed tower diameter is determined according to HCl treating capacity, and HCl gas flow velocity in tower is 0.2 ~ 1.0m/s;
(2) second level is watery hydrochloric acid system, and watery hydrochloric acid tower circulation watery hydrochloric acid concentration is 15 ~ 20%, temperature 10 ~ 20 DEG C, internal circulating load 3 ~ 15m3/h; Watery hydrochloric acid adopts continuous feeding and discharging mode, and the watery hydrochloric acid groove of watery hydrochloric acid absorption system flows into concentrated hydrochloric acid groove by liquid level difference continuously;
(3) third level is weak hydrochloric acid system, and weak hydrochloric acid groove utilizes liquid level difference to continuously flow into watery hydrochloric acid groove, and the weak hydrochloric acid tower cyclic absorption concentration of weak hydrochloric acid absorption system is 5 ~ 10%, temperature 10 ~ 20 DEG C, internal circulating load 3 ~ 15m3/h; Weak hydrochloric acid adopts continuous feeding and discharging mode, and the weak hydrochloric acid groove of weak hydrochloric acid absorption system flows into watery hydrochloric acid groove by liquid level difference continuously;
(4) fourth stage is water wash system, and water scrubber circulating absorption solution is 1 ~ 5% containing HCl concentration, absorbs temperature 10 ~ 20 DEG C, internal circulating load 3 ~ 15m3/h; Water wash system adopts continuous running water to add to rinsing bowl, and keeps the liquid level of rinsing bowl, and water magnitude of recruitment is determined by HCl is gas generated;
(5) level V is caustic washing system, and lye tank (vat) abNaOH concentration is 2 ~ 5%, alkali cleaning internal circulating load 3 ~ 15m3/h, alkali cleaning temperature 10 ~ 20 DEG C; Lye tank (vat) has two can carry out handover operation, will switch when alkali wash water reaches pH8, prevents HCl gas from entering vacuum suction unit, causes unit acidity to destroy.
2. the HCl Gas recovering method under a kind of high vacuum condition according to claim 1, is characterized in that: concentrated hydrochloric acid tower cyclic absorption HCl gas concentration preferably 31% in the described first order, temperature preferably 15 DEG C, the preferred 10m3/h of internal circulating load.
3. the HCl Gas recovering method under a kind of high vacuum condition according to claim 1, is characterized in that: the preferred 0.5m/s of HCl gas flow velocity in tower in the described first order.
4. the HCl Gas recovering method under a kind of high vacuum condition according to claim 1, is characterized in that: watery hydrochloric acid tower circulation watery hydrochloric acid concentration preferably 18% in the described second level, temperature preferably 15 DEG C, the preferred 10m3/h of internal circulating load.
5. the HCl Gas recovering method under a kind of high vacuum condition according to claim 1, is characterized in that: the weak hydrochloric acid tower cyclic absorption concentration of absorption by Hydrochloric Acid system preferably 8% in the described third level, temperature preferably 15 DEG C, the preferred 10m3/h of internal circulating load.
6. the HCl Gas recovering method under a kind of high vacuum condition according to claim 1, is characterized in that: in the described fourth stage, water scrubber circulating absorption solution is containing HCl concentration preferably 2%, absorbs temperature preferably 15 DEG C, the preferred 10m3/h of internal circulating load.
7. the HCl Gas recovering method under a kind of high vacuum condition according to claim 1, is characterized in that: lye tank (vat) abNaOH concentration preferably 3%, the preferred 10m3/h of alkali cleaning internal circulating load in described level V, alkali cleaning temperature preferably 15 DEG C.
8. the HCl Gas recovering method under a kind of high vacuum condition according to claim 1, is characterized in that: described concentrated hydrochloric acid tower, watery hydrochloric acid tower, weak hydrochloric acid tower, water scrubber and caustic wash tower adopt packed tower, select the filler that specific area is large, efficiency is high.
9. the HCl Gas recovering method under a kind of high vacuum condition according to claim 8, is characterized in that: the preferred 4m of described filler in packed column height, the preferred regular polypropylene version ripple packing of packed tower.
10. the HCl Gas recovering method under a kind of high vacuum condition according to claim 9, is characterized in that: the difference in height between bottom described annular groove top and packed tower is greater than 12m.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106362555A (en) * | 2016-09-12 | 2017-02-01 | 江苏必康制药股份有限公司 | Process gas purification treatment method |
| CN108926961A (en) * | 2018-07-25 | 2018-12-04 | 乳源东阳光氟树脂有限公司 | A kind of hydrogen chloride water washing cycles absorption system and its application |
| CN109264672A (en) * | 2018-11-13 | 2019-01-25 | 乳源东阳光氟树脂有限公司 | A kind of hydrogen chloride water absorption system and its application |
| CN110813064A (en) * | 2019-12-10 | 2020-02-21 | 遵宝钛业有限公司 | Method for comprehensively treating chlorine-containing tail gas in production of titanium tetrachloride through boiling chlorination |
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| CN201324588Y (en) * | 2008-12-08 | 2009-10-14 | 江阴苏利化学有限公司 | Hydrogen chloride gas absorption system |
| CN101658758A (en) * | 2008-08-29 | 2010-03-03 | 四川省乐山市福华通达农药科技有限公司 | Method for removing hydrogen chloride in chemically synthesized tail gas |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101658758A (en) * | 2008-08-29 | 2010-03-03 | 四川省乐山市福华通达农药科技有限公司 | Method for removing hydrogen chloride in chemically synthesized tail gas |
| CN201324588Y (en) * | 2008-12-08 | 2009-10-14 | 江阴苏利化学有限公司 | Hydrogen chloride gas absorption system |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106362555A (en) * | 2016-09-12 | 2017-02-01 | 江苏必康制药股份有限公司 | Process gas purification treatment method |
| CN106362555B (en) * | 2016-09-12 | 2019-06-28 | 江苏九九久科技有限公司 | Process gas purifying treatment method |
| CN108926961A (en) * | 2018-07-25 | 2018-12-04 | 乳源东阳光氟树脂有限公司 | A kind of hydrogen chloride water washing cycles absorption system and its application |
| CN109264672A (en) * | 2018-11-13 | 2019-01-25 | 乳源东阳光氟树脂有限公司 | A kind of hydrogen chloride water absorption system and its application |
| CN110813064A (en) * | 2019-12-10 | 2020-02-21 | 遵宝钛业有限公司 | Method for comprehensively treating chlorine-containing tail gas in production of titanium tetrachloride through boiling chlorination |
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Application publication date: 20150617 |