CN103933831B - A kind of recovery method producing ammonia in 4-5 amido benzotrifluoride technique - Google Patents
A kind of recovery method producing ammonia in 4-5 amido benzotrifluoride technique Download PDFInfo
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- CN103933831B CN103933831B CN201410161583.6A CN201410161583A CN103933831B CN 103933831 B CN103933831 B CN 103933831B CN 201410161583 A CN201410161583 A CN 201410161583A CN 103933831 B CN103933831 B CN 103933831B
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Abstract
The invention discloses a kind of recovery method producing ammonia in 4-5 amido benzotrifluoride technique, the method comprises the following steps: tail is inhaled ammoniacal liquor and inject vavuum pump water tank, stage falling-film absorption cell is added fresh water (FW), clear water is added in secondary falling film absorption groove, fresh water (FW), open tertiary effluent spray absorber, open stage falling-film absorption tower and secondary film-falling absorption tower, to the ammoniacal liquor sampling censorship of cyclic absorption, Ammonia vessel is pumped to wash expects that washing of post expects ammoniacal liquor head tank, if when having ammoniacal liquor to need export trade, after sampling censorship, can directly pump in export trade ammonia vessel tank car from Ammonia vessel.Beneficial effect: while the useful material of recycling, greatly reduce the discharge of ammonia exhaust gas, so both decreased the pollution to environment, turn increased economic benefit.
Description
Technical field
The present invention relates to 4-5 amido benzotrifluoride technique, particularly relate to a kind of recovery method producing ammonia in 4-5 amido benzotrifluoride technique.
Background technology
For a long time, in production 4-5 amido benzotrifluoride technique, to take liquefied ammonia as raw material during ammonification, a large amount of ammonias can be produced during reaction decomposes, former technique is directly emptying after taking simple measure to this, not only causes larger pollution to environment, also wastes resource (ammonia) greatly.And ammonia is very easily water-soluble, tail ammonia water can be considered to absorb, convert to relative to storing ammoniacal liquor easily, ammoniacal liquor can use as workshop raw material (washing material post), also can directly export trade, the pollution to environment can be reduced like this, can economic benefit be obtained again, thus impel the enforcement of this programme.Therefore, for solving the problem, spy provides a kind of new technical scheme.
Summary of the invention
The invention provides a kind of recovery method producing ammonia in 4-5 amido benzotrifluoride technique.
The technical solution used in the present invention: in a kind of 4-of production 5 amido benzotrifluoride technique, the recovery method of ammonia comprises the following steps:
(1) tail is inhaled ammoniacal liquor and inject vavuum pump water tank, stage falling-film absorption cell is added fresh water (FW) to 3/4 of liquid level visor, clear water is added to 3/4 of liquid level visor in secondary falling film absorption groove, secondary falling film absorption groove is without weak aqua ammonia, also add fresh water (FW) to 3/4 of liquid level visor, open the recirculated water turnover valve of tertiary effluent spray absorber;
(2) after the notice pressure release of high-pressure synthesis post, binder, open the chilled brine turnover valve on stage falling-film absorption tower and the recirculated water turnover valve of secondary film-falling absorption tower, stage falling-film absorption tower and secondary film-falling absorption tower is made to carry out the cyclic absorption of ammoniacal liquor with stage falling-film absorption cell, secondary falling film absorption groove respectively, until precipitation post precipitation terminates, after cooling reaches 100-110 DEG C, stop the cyclic absorption of ammoniacal liquor, close the chilled brine turnover valve on stage falling-film absorption tower and the recirculated water turnover valve of secondary film-falling absorption tower;
(3) to the ammoniacal liquor sampling censorship of cyclic absorption, control ammonia concn≤8% of secondary falling film absorption groove, the ammonia concn of stage falling-film absorption cell is between 20-22%;
(4) after the ammonia concn of secondary falling film absorption groove reaches 6-8%, pump into stage falling-film absorption cell, when ammonia concn >=4% of vavuum pump water tank, pump into secondary falling film absorption groove; The water of tertiary effluent spray absorber feeds Water spray and absorbs receiving slit, and when adding the liquid level of fresh water (FW) to 3/4 and the Water spray absorption receiving slit of visor in vavuum pump water tank and reaching 3/4, pumps into secondary falling film absorption groove;
(5) when the ammonia concn of stage falling-film absorption cell reaches 20%, pump into Ammonia vessel, mend ammoniacal liquor that secondary falling film absorption groove absorbs or the sewage disposal weak aqua ammonia 1/2-3/4 to tank liquor position in stage falling-film absorption cell;
(6) wash material post when needing to wash material ammoniacal liquor, by Ammonia vessel be pumped to wash material post wash material ammoniacal liquor head tank, calculate actual ammonia volume according to censorship ammonia concn, wash material ammoniacal liquor for every batch and amount to 22% ammoniacal liquor 200kg;
(7) if when having ammoniacal liquor to need export trade, after sampling censorship, directly pump in export trade ammonia vessel tank car from Ammonia vessel.
The material of above-mentioned stage falling-film absorption tower and secondary film-falling absorption tower is graphite.
Beneficial effect of the present invention: it is graphite material that tail ammonia absorbs the film-falling absorption tower adopted, has the advantages such as absorption efficiency is high, corrosion-resistant, absorption intensity is high, product ammonia concn is high, outlet temperature is low, stable operation, control convenience; While the useful material of recycling, greatly reduce the discharge of ammonia exhaust gas; Ammonia effect is absorbed better by water circulation, ammonia is after two-stage falling film absorption, the absorption efficiency of ammonia reaches more than 99%, for preventing small part unabsorbed tail ammonia uncontrollable discharge, after secondary falling film absorption, adopt tertiary effluent spray-absorption again, finally discharged ammonia emission concentration and rate of discharge are far below its corresponding discharge standard, so both decrease the pollution to environment, turn increase economic benefit.
Accompanying drawing explanation
Fig. 1 is that flow process of the present invention is shown in figure.
Detailed description of the invention
As shown in Figure 1, in a kind of 4-of production 5 amido benzotrifluoride technique, the recovery method of ammonia comprises the following steps:
(1) tail is inhaled ammoniacal liquor and inject vavuum pump water tank, stage falling-film absorption cell is added fresh water (FW) to 3/4 of liquid level visor, clear water is added to 3/4 of liquid level visor in secondary falling film absorption groove, secondary falling film absorption groove is without weak aqua ammonia, also add fresh water (FW) to 3/4 of liquid level visor, open the recirculated water turnover valve of tertiary effluent spray absorber;
(2) after the notice pressure release of high-pressure synthesis post, binder, open the chilled brine turnover valve on stage falling-film absorption tower and the recirculated water turnover valve of secondary film-falling absorption tower, stage falling-film absorption tower and secondary film-falling absorption tower is made to carry out the cyclic absorption of ammoniacal liquor with stage falling-film absorption cell, secondary falling film absorption groove respectively, until precipitation post precipitation terminates, after cooling reaches 100-110 DEG C, stop the cyclic absorption of ammoniacal liquor, close the chilled brine turnover valve on stage falling-film absorption tower and the recirculated water turnover valve of secondary film-falling absorption tower;
(3) to the ammoniacal liquor sampling censorship of cyclic absorption, control ammonia concn≤8% of secondary falling film absorption groove, the ammonia concn of stage falling-film absorption cell is between 20-22%;
(4) after the ammonia concn of secondary falling film absorption groove reaches 6-8%, pump into stage falling-film absorption cell, when ammonia concn >=4% of vavuum pump water tank, pump into secondary falling film absorption groove; The water of tertiary effluent spray absorber feeds Water spray and absorbs receiving slit, and when adding the liquid level of fresh water (FW) to 3/4 and the Water spray absorption receiving slit of visor in vavuum pump water tank and reaching 3/4, pumps into secondary falling film absorption groove;
(5) when the ammonia concn of stage falling-film absorption cell reaches 20%, pump into Ammonia vessel, mend ammoniacal liquor that secondary falling film absorption groove absorbs or the sewage disposal weak aqua ammonia 1/2-3/4 to tank liquor position in stage falling-film absorption cell;
(6) wash material post when needing to wash material ammoniacal liquor, by Ammonia vessel be pumped to wash material post wash material ammoniacal liquor head tank, calculate actual ammonia volume according to censorship ammonia concn, wash material ammoniacal liquor for every batch and amount to 22% ammoniacal liquor 200kg;
(7) if when having ammoniacal liquor to need export trade, after sampling censorship, directly pump in export trade ammonia vessel tank car from Ammonia vessel.
The material of above-mentioned stage falling-film absorption tower and secondary film-falling absorption tower is graphite.
Beneficial effect: it is graphite material that tail ammonia absorbs the film-falling absorption tower adopted, has the advantages such as absorption efficiency is high, corrosion-resistant, absorption intensity is high, product ammonia concn is high, outlet temperature is low, stable operation, control convenience; While the useful material of recycling, greatly reduce the discharge of ammonia exhaust gas; Ammonia effect is absorbed better by water circulation, ammonia is after two-stage falling film absorption, the absorption efficiency of ammonia reaches more than 99%, for preventing small part unabsorbed tail ammonia uncontrollable discharge, after secondary falling film absorption, adopt tertiary effluent spray-absorption again, finally discharged ammonia emission concentration and rate of discharge are far below its corresponding discharge standard, so both decrease the pollution to environment, turn increase economic benefit.
Claims (2)
1. produce a recovery method for ammonia in 4-5 amido benzotrifluoride technique, it is characterized in that comprising the following steps:
(1) tail is inhaled ammoniacal liquor and inject vavuum pump water tank, stage falling-film absorption cell is added fresh water (FW) to 3/4 of liquid level visor, clear water is added to 3/4 of liquid level visor in secondary falling film absorption groove, secondary falling film absorption groove also adds fresh water (FW) to 3/4 of liquid level visor without weak aqua ammonia, opens the recirculated water turnover valve of tertiary effluent spray absorber;
(2) after the notice pressure release of high-pressure synthesis post, binder, open the chilled brine turnover valve on stage falling-film absorption tower and the recirculated water turnover valve of secondary film-falling absorption tower, stage falling-film absorption tower and secondary film-falling absorption tower is made to carry out the cyclic absorption of ammoniacal liquor with stage falling-film absorption cell, secondary falling film absorption groove respectively, until precipitation post precipitation terminates, after cooling reaches 100-110 DEG C, stop the cyclic absorption of ammoniacal liquor, close the chilled brine turnover valve on stage falling-film absorption tower and the recirculated water turnover valve of secondary film-falling absorption tower;
(3) to the ammoniacal liquor sampling censorship of cyclic absorption, control ammonia concn≤8% of secondary falling film absorption groove, the ammonia concn of stage falling-film absorption cell is between 20-22%;
(4) after the ammonia concn of secondary falling film absorption groove reaches 6-8%, pump into stage falling-film absorption cell, when ammonia concn >=4% of vavuum pump water tank, pump into secondary falling film absorption groove; The water of tertiary effluent spray absorber feeds Water spray and absorbs receiving slit, and when adding the liquid level of fresh water (FW) to 3/4 and the Water spray absorption receiving slit of visor in vavuum pump water tank and reaching 3/4, pumps into secondary falling film absorption groove;
(5) when the ammonia concn of stage falling-film absorption cell reaches 20%, pump into Ammonia vessel, mend the ammoniacal liquor of secondary falling film absorption groove or the sewage disposal weak aqua ammonia 1/2-3/4 to tank liquor position in stage falling-film absorption cell;
(6) wash material post when needing to wash material ammoniacal liquor, by Ammonia vessel be pumped to wash material post wash material ammoniacal liquor head tank, calculate actual ammonia volume according to censorship ammonia concn, wash material ammoniacal liquor for every batch and amount to 22% ammoniacal liquor 200kg;
(7) if when having ammoniacal liquor to need export trade, after sampling censorship, directly pump in export trade ammonia vessel tank car from Ammonia vessel.
2. a kind of recovery method producing ammonia in 4-5 amido benzotrifluoride technique according to claim 1, is characterized in that: the material of described stage falling-film absorption tower and secondary film-falling absorption tower is graphite.
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| CN104117267A (en) * | 2014-08-11 | 2014-10-29 | 乳山市日晟机械制造有限公司 | Ammonia gas film-falling absorption device |
| CN106215449B (en) * | 2016-08-29 | 2018-11-16 | 石家庄杰克化工有限公司 | A kind of 4,6- dihydroxy-pyrimidine reaction system tail gas treatment process |
| CN109173606A (en) * | 2018-09-21 | 2019-01-11 | 海宁市英德赛电子有限公司 | A kind of ammonia-containing exhaust processing system and treatment process |
| CN108970341A (en) * | 2018-10-15 | 2018-12-11 | 广东宏昊化工有限公司 | A kind of exhaust treatment system recycling high concentration ammonium hydroxide from ammonia-containing exhaust |
| CN114436459A (en) * | 2020-10-30 | 2022-05-06 | 伊斯拓通用设备江苏有限公司 | Method for treating wastewater discharged by ammonium fluoride production process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2239030A1 (en) * | 2009-04-08 | 2010-10-13 | Sturla, Vittorio | A process for stripping and recovering ammonia from digested wastes and plant for carrying out said process. |
| CN102179134A (en) * | 2011-04-26 | 2011-09-14 | 苏州利盛化工设备有限公司 | Ammonia water recovery device |
| CN202237350U (en) * | 2011-10-09 | 2012-05-30 | 常州寅盛药业有限公司 | Three-stage ammonia gas absorbing system |
| CN102772982A (en) * | 2011-05-12 | 2012-11-14 | 特力生有限公司 | Method for recycling ammonia gas |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2239030A1 (en) * | 2009-04-08 | 2010-10-13 | Sturla, Vittorio | A process for stripping and recovering ammonia from digested wastes and plant for carrying out said process. |
| CN102179134A (en) * | 2011-04-26 | 2011-09-14 | 苏州利盛化工设备有限公司 | Ammonia water recovery device |
| CN102772982A (en) * | 2011-05-12 | 2012-11-14 | 特力生有限公司 | Method for recycling ammonia gas |
| CN202237350U (en) * | 2011-10-09 | 2012-05-30 | 常州寅盛药业有限公司 | Three-stage ammonia gas absorbing system |
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