CN109626330B - Distillation recovery device and method for hydrogen chloride in acidic etching waste liquid - Google Patents
Distillation recovery device and method for hydrogen chloride in acidic etching waste liquid Download PDFInfo
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- CN109626330B CN109626330B CN201910045614.4A CN201910045614A CN109626330B CN 109626330 B CN109626330 B CN 109626330B CN 201910045614 A CN201910045614 A CN 201910045614A CN 109626330 B CN109626330 B CN 109626330B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
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Abstract
The invention discloses a distillation recovery device of hydrogen chloride in acidic etching waste liquid, which comprises a reaction kettle (1) and a circulating absorption system, wherein a stirring motor (4), a temperature detector (3), an etching liquid inlet (2) and an etching liquid outlet (38) are arranged on the reaction kettle (1); the circulating absorption system comprises a primary absorption tower (8), a secondary absorption tower (12) and a tertiary absorption tower (17), and a condenser A (7), a condenser B (11) and a condenser C (15) are respectively and fixedly arranged on the primary absorption tower (8), the secondary absorption tower (12) and the tertiary absorption tower (17); each absorption tower is provided with a pump and a valve, and the absorption towers are connected through a pipeline to realize the transfer of acid liquor so as to gradually increase the concentration of hydrochloric acid; the invention has the beneficial effects that: by utilizing the distillation of the reaction kettle and the circulating absorption of the multi-stage recovery tower, the low-concentration hydrochloric acid solution can be further transferred to other absorption towers to increase the recovery efficiency, the recovery cost is low, and no new harmful substances are added and generated.
Description
Technical Field
The invention relates to the field of industrial wastewater treatment, in particular to a distillation recovery device and a method for hydrogen chloride in acidic etching waste liquid.
Background
A large amount of hydrochloric acid-containing wastewater is discharged from a PCB (printed circuit board) etching production line, and if conventional treatment is adopted, alkali is needed for neutralization and then desalting treatment, so that a large amount of alkali is consumed, a large amount of salt is generated, and the hydrochloric acid is too low in concentration and cannot be recycled, so that direct discharge is not beneficial to environmental protection and cost saving.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a device and a method for recovering hydrogen chloride in etching waste liquid, which adopt distillation mode for multi-stage circulating absorption, have low cost and do not need to add medicaments.
The purpose of the invention is realized by the following technical scheme: a distillation recovery device for hydrogen chloride in acidic etching waste liquid comprises a reaction kettle and a circulating absorption system, wherein the reaction kettle is provided with a stirring motor, a temperature detector, an etching liquid inlet and an etching liquid outlet; the circulating absorption system comprises a primary absorption tower, a secondary absorption tower and a tertiary absorption tower, wherein a condenser A, a condenser B and a condenser C are respectively arranged on the primary absorption tower, the secondary absorption tower and the tertiary absorption tower; the reaction kettle is connected with a condenser A through a pipeline A, and the condenser A is connected with the lower part of the primary absorption tower through a pipeline B; the primary absorption tower is connected with a condenser B through a pipeline C; the condenser B is connected with the lower part of the secondary absorption tower through a pipeline D; the secondary absorption tower is connected with a condenser C through a pipeline E, and the condenser C is connected with the lower part of the tertiary absorption tower through a pipeline F.
Furthermore, the reaction kettle is an enamel reaction kettle, and a heat source in the reaction kettle is provided by a heat conduction oil furnace.
Furthermore, valves are arranged on the etching liquid inlet, the etching liquid outlet and the pipeline A.
Furthermore, all be provided with valve and pump on pipeline B, pipeline D and the pipeline F, be provided with pump A and valve B on the pipeline B promptly, be provided with pump B and valve F on the pipeline D, be provided with pump C and valve i on the pipeline F.
Furthermore, a hydrochloric acid liquid outlet is also arranged at the lower part of the primary absorption tower, and a valve a is arranged on the hydrochloric acid liquid outlet.
Furthermore, a clear water inlet is formed in the lower portion of the tertiary absorption tower, and a valve h is arranged on the clear water inlet.
Furthermore, the pipeline B is connected with a pipeline G through a tee joint at one section between the condenser A and the pump A, the other end of the pipeline G is connected with a sulfuric acid outlet, and a valve d is arranged on the pipeline G.
Furthermore, pipeline D has pipeline H through tee junction on lieing in one section between condenser B and pump B, and the pipeline H other end adopts tee junction to lie in the pipeline B between the section between valve B and the pump A, is provided with valve g on the pipeline H.
Furthermore, a section of the pipeline F between the condenser C and the pump C is connected with a pipeline I through a tee joint, the other end of the pipeline I is connected with the bottom of the secondary absorption tower, and a valve j is arranged on the pipeline I.
A distillation recovery method of hydrogen chloride in acidic etching waste liquid is characterized by comprising the following steps: it comprises the following steps:
s1, introducing etching waste liquid into a reaction kettle, introducing heat conduction oil to heat and keeping the temperature of the etching waste liquid in the reaction kettle within the range of 105-115 ℃; simultaneously, clear water with the volume of 1/3 of the absorption tower is introduced into each absorption tower;
s2, starting a stirring motor to carry out distillation stirring, and separating out a mixed gas containing hydrogen chloride gas and water vapor from the etching waste liquid;
s3, when the temperature of the mixed gas in the reaction kettle reaches 45-50 ℃, opening a valve arranged on the pipeline A, and enabling the mixed gas to enter the condenser A and enter the primary absorption tower along the spraying pipe for absorption; residual gas separated out from the primary absorption tower enters a secondary absorption tower along a pipeline C for absorption, and residual gas separated out from the secondary absorption tower enters a tertiary absorption tower along a pipeline E for absorption;
s4, when the concentration of the hydrogen chloride in the hydrochloric acid solution in the primary absorption tower reaches a preset standard, opening a valve a to discharge the hydrochloric acid in the primary absorption tower into a finished product tank along a hydrochloric acid liquid outlet; opening a valve f, a valve g, a valve c and a valve B, and pumping the hydrochloric acid solution in the secondary absorption tower into the primary absorption tower along a pipeline H by a pump B; opening a valve I, a valve j and a valve e, pumping the hydrochloric acid solution in the tertiary absorption tower into the secondary absorption tower along a pipeline I by a pump C, and completing the rotation of the hydrochloric acid solution in the primary absorption tower and the secondary absorption tower;
s5, after the hydrochloric acid in the tertiary absorption tower is transferred, opening a valve h on a clear water inlet, and introducing clear water into the tertiary absorption tower;
and S6, after the concentration of the hydrochloric acid in the etching waste liquid distilled in the reaction kettle is reduced to a preset standard, discharging and discharging the etching waste liquid from an etching liquid outlet, and storing the etching waste liquid for other production processes.
The invention has the following advantages:
by adopting a physical method, the distillation of the reaction kettle and the cyclic absorption of the multi-stage recovery tower are utilized, the low-concentration hydrochloric acid solution can be further transferred to other absorption towers to increase the recovery efficiency, the recovery cost is low, and no new harmful substance is added and generated.
Drawings
FIG. 1 is a schematic structural view of the present invention;
in the figure: 1-a reaction kettle, 2-an etching solution inlet, 3-a temperature detector, 4-a stirring motor, 5-a pipeline A, 6-a pipeline B, 7-a condenser A, 8-a primary absorption tower, 9-a pipeline C, 10-a pipeline D, 11-a condenser B, 12-a secondary absorption tower, 13-a pipeline E, 14-a pipeline F, 15-a condenser C, 16-an exhaust port, 17-a tertiary absorption tower, 18-a spray pipe, 19-a valve j, 20-a pipeline I, 21-a pump C, 22-a valve I, 23-a clear water inlet, 24-a valve H, 25-a valve G, 26-a pump B, 27-a valve F, 28-a pipeline H, 29-a valve E, 30-a valve D, 31-a pump A, 32-a valve C, 33-a valve B, 34-a pipeline G, 35-a valve a, 36-a hydrochloric acid liquid outlet, 37-a stirring blade and 38-an etching solution outlet.
Detailed Description
The invention will be further described with reference to the accompanying drawings, but the scope of the invention is not limited to the following.
As shown in fig. 1, a distillation recovery device for hydrogen chloride in acidic waste etching solution comprises a reaction kettle 1 and a circulating absorption system, wherein the reaction kettle 1 is provided with a stirring motor 4, a temperature detector 3, an etching solution inlet 2 and an etching solution outlet 38, the temperature detector 3 is provided with two groups, one group is used for detecting the temperature of the waste etching solution, and the other group is used for detecting the temperature of gas in the reaction kettle 1; stirring motor 4 is connected with stirring vane 37 through the transmission shaft, and stirring vane 37 is located reation kettle 1 inside.
The circulating absorption system comprises a primary absorption tower 8, a secondary absorption tower 12 and a tertiary absorption tower 17, wherein a condenser A7, a condenser B11 and a condenser C15 are respectively arranged on the primary absorption tower 8, the secondary absorption tower 12 and the tertiary absorption tower 17; the top of the reaction kettle 1 is provided with a pipeline A5, the other end of the pipeline A5 is connected with a condenser A7, the condenser A7 is connected with the lower part of a primary absorption tower 8 through a pipeline B6, the lower part of the primary absorption tower 8 is provided with a hydrochloric acid liquid outlet 36, and the hydrochloric acid liquid outlet 36 is provided with a valve a35; a pump A31 and a valve B33 are arranged on the pipeline B6, a section of the pipeline B6, which is positioned between the condenser A7 and the pump A31, is connected with a pipeline G34 through a tee joint, the other end of the pipeline G34 is connected with a hydrochloric acid liquid outlet 36 through a tee joint, and a valve d30 is arranged on the pipeline G34; the primary absorption tower 8 is connected with a condenser B11 through a pipeline C9, and the condenser B11 is connected with the lower part of a secondary absorption tower 12 through a pipeline D10; a pump B26 and a valve f27 are arranged on the pipeline D10, a pipeline H28 is further connected to one section of the pipeline D10, which is positioned between the condenser B11 and the pump B26, through a tee joint, the other end of the pipeline H28 is connected to a pipeline B6, which is positioned between a valve B33 and a pump A31, through a tee joint, and a valve g25 and a valve c32 are arranged on the pipeline H28; the secondary absorption tower 12 is connected with a condenser C15 through a pipeline E13, and the condenser C15 is connected with the lower part of a tertiary absorption tower 17 through a pipeline F14; a pump C21 and a valve I22 are arranged on the pipeline F14, a section of the pipeline F14, which is positioned between the condenser C15 and the pump C21, is connected with a pipeline I20 through a tee joint, the other end of the pipeline I20 is connected with the bottom of the secondary absorption tower 12, and a valve j19 and a valve e29 are arranged on the pipeline I20; an exhaust port 16 is formed in the upper portion of the tertiary absorption tower 17, a clear water inlet 23 is formed in the lower portion of the tertiary absorption tower 17, and a valve h24 is arranged on the clear water inlet 23.
The reaction kettle 1 is an enamel reaction kettle, and a heat source in the reaction kettle 1 is provided by a heat conduction oil furnace; the condenser A7, the condenser B11 and the condenser C15 are fixedly connected with spray pipes 18, and the tail ends of the spray pipes 18 extend into the primary absorption tower 8, the secondary absorption tower 12 and the tertiary absorption tower 17; valves are arranged on the etching solution inlet 2, the etching solution outlets and 38 and the pipeline A5 to control the flow.
A method for distilling and recovering hydrogen chloride in acidic etching waste liquid is characterized by comprising the following steps: the method comprises the following steps:
s1, introducing the etching waste liquid into a reaction kettle 1 along an etching liquid inlet 2, heating by using heat conduction oil, and keeping the temperature of the etching waste liquid in the reaction kettle 1 within the range of 105-115 ℃; simultaneously opening a valve H24, a valve I22, a valve j19, a valve e29, a valve F27, a valve g25, a valve C32 and a valve B33, under the work of a pump C21, a pump B26 and a pump A31, clear water enters the tertiary absorption tower 17 along a clear water inlet 23, sequentially enters the secondary absorption tower 12 along a pipeline I20, enters the primary absorption tower 8 along a pipeline H28, and circularly sprays between the tower bottom and the tower top of each absorption tower along a pipeline B6, a pipeline D10 and a pipeline F14 respectively; the amount of the clean water introduced into the primary absorption tower 8, the secondary absorption tower 12 and the tertiary absorption tower 17 is 1/3 of the volume of the clean water and submerges the tail end of the spray pipe 18; when the clean water is introduced, closing the valve;
s2, starting a stirring motor 4 to carry out distillation stirring, and separating out a mixed gas containing hydrogen chloride gas and water vapor from the etching waste liquid;
s3, when the temperature of the mixed gas in the reaction kettle reaches 45-50 ℃, opening a valve arranged on a pipeline A5, and allowing the mixed gas to enter a condenser A7 and enter a primary absorption tower 8 along a spray pipe 18 for absorption; residual gas separated out from the primary absorption tower 8 enters a secondary absorption tower 12 to be absorbed along a pipeline C9 and a condenser B11, residual gas separated out from the secondary absorption tower 12 enters a tertiary absorption tower 17 to be absorbed along a pipeline E13 and a condenser C15, the concentration of hydrochloric acid formed by absorbing hydrogen chloride in each absorption tower is reduced in sequence, and residual tail gas is discharged into other collection processing procedures along an exhaust port 16;
s4, when the concentration of the hydrogen chloride in the hydrochloric acid solution in the primary absorption tower 8 reaches a preset standard, opening a valve a35, and discharging the hydrochloric acid in the primary absorption tower 8 into a finished product tank along a hydrochloric acid liquid outlet 35; opening a valve f27, a valve g25, a valve c32 and a valve B33, and pumping the hydrochloric acid solution in the secondary absorption tower 12 into the primary absorption tower 8 along a pipeline H28 by a pump B26; opening a valve I22, a valve j19 and a valve e29, pumping the hydrochloric acid solution in the tertiary absorption tower 17 into the secondary absorption tower 12 along a pipeline I20 through a pump C21, and completing the rotation of the acid solution in the primary absorption tower 8 and the secondary absorption tower 12;
s5, after the hydrochloric acid in the tertiary absorption tower 17 is transferred, opening a valve h24 on a clear water inlet 23, and introducing clear water into the tertiary absorption tower 17;
s6, after the concentration of the hydrochloric acid in the etching waste liquid distilled in the reaction kettle 1 is reduced to a preset standard, discharging and discharging the etching waste liquid from an etching liquid outlet 38, and storing the etching waste liquid for other production processes.
The concentration of the hydrochloric acid in the etching solution is different, the boiling point temperature during distillation is also different, in the embodiment, the boiling point of the hydrochloric acid solution is 110 ℃, and the concentration of the hydrochloric acid solution generated after distillation by adopting the device and the method can reach more than 25%, so that the recycling concentration of the hydrochloric acid required in the regeneration of the etching solution is met.
Claims (6)
1. A distillation recovery device of hydrogen chloride in acid etching waste liquid is characterized in that: the device comprises a reaction kettle (1) and a circulating absorption system, wherein a stirring motor (4), a temperature detector (3), an etching solution inlet (2) and an etching solution outlet (38) are arranged on the reaction kettle (1); the circulating absorption system comprises a primary absorption tower (8), a secondary absorption tower (12) and a tertiary absorption tower (17), and a condenser A (7), a condenser B (11) and a condenser C (15) are respectively and fixedly arranged on the primary absorption tower (8), the secondary absorption tower (12) and the tertiary absorption tower (17); the reaction kettle (1) is connected with a condenser A (7) through a pipeline A (5), and the condenser A (7) is connected with the lower part of a primary absorption tower (8) through a pipeline B (6); the primary absorption tower (8) is connected with a condenser B (11) through a pipeline C (9); the condenser B (11) is connected with the lower part of the secondary absorption tower (12) through a pipeline D (10); the secondary absorption tower (12) is connected with a condenser C (15) through a pipeline E (13), and the condenser C (15) is connected with the lower part of the tertiary absorption tower (17) through a pipeline F (14);
the pipeline B (6) is provided with a pump A (31) and a valve B (33); a pump B (26) and a valve f (27) are arranged on the pipeline D (10); a pump C (21) and a valve i (22) are arranged on the pipeline F (14); a hydrochloric acid liquid outlet (36) is formed in the lower portion of the primary absorption tower (8), and a valve a (35) is arranged on the hydrochloric acid liquid outlet (36); a clear water inlet (23) is formed in the lower portion of the tertiary absorption tower (17), and a valve h (24) is arranged on the clear water inlet (23);
a section of the pipeline B (6) between the condenser A (7) and the pump A (31) is in three-way connection with a pipeline G (34), the other end of the pipeline G (34) is in three-way connection with a hydrochloric acid liquid outlet (36), and a valve d (30) is arranged on the pipeline G (34); the pipeline D (10) is also connected with a pipeline H (28) through a tee joint at one section between the condenser B (11) and the pump B (26), the other end of the pipeline H (28) is connected with a pipeline B (6) between the valve B (33) and the pump A (31) through a tee joint, and the pipeline H (28) is provided with a valve g (25) and a valve c (32); a section of the pipeline F (14) between the condenser C (15) and the pump C (21) is connected with a pipeline I (20) through a tee joint, the other end of the pipeline I (20) is connected with the bottom of the secondary absorption tower (12), and a valve j (19) and a valve e (29) are arranged on the pipeline I (20);
the method comprises the following steps:
s1, feeding etching waste liquid with volume of 75% into a reaction kettle (1) along an etching liquid inlet (2), introducing heat conduction oil for heating, and keeping the temperature of the etching waste liquid in the reaction kettle within the range of 105-115 ℃; simultaneously, clear water with the volume of 1/3 is introduced into the absorption towers;
s2, starting a stirring motor (4) to carry out distillation stirring, and separating out a mixed gas containing hydrogen chloride gas and water vapor from the etching waste liquid;
s3, when the temperature of the mixed gas in the reaction kettle (1) reaches 45-50 ℃, opening a valve arranged on a pipeline A (5), allowing the mixed gas to enter a condenser A (7) and enter a primary absorption tower (8) along a spray pipe for absorption; residual gas separated out from the primary absorption tower (8) enters a secondary absorption tower (12) along a pipeline C (9) for absorption, and residual gas separated out from the secondary absorption tower (12) enters a tertiary absorption tower (17) along a pipeline E (13) for absorption;
s4, when the concentration of hydrogen chloride in the hydrochloric acid solution in the primary absorption tower (8) reaches a preset standard, opening a valve a (35), and discharging the hydrochloric acid in the primary absorption tower (8) into a finished product tank along a hydrochloric acid liquid outlet (36); opening a valve f (27), a valve g (25), a valve c (32) and a valve B (32), pumping the hydrochloric acid solution in the secondary absorption tower (12) into the primary absorption tower (8) along a pipeline H (28) through a pump B (26); opening a valve I (22), a valve j (19) and a valve e (29), pumping the hydrochloric acid solution in the tertiary absorption tower (17) into the secondary absorption tower (12) along a pipeline I (20) through a pump C (21), and completing the rotation of the hydrochloric acid solution in the primary absorption tower (8) and the secondary absorption tower (12);
s5, after the hydrochloric acid in the tertiary absorption tower (17) is transferred, opening a valve h (24) on a clear water inlet (23) to introduce clear water into the tertiary absorption tower (18);
and S6, after the concentration of the hydrochloric acid in the etching waste liquid distilled in the reaction kettle is reduced to a preset standard, discharging (38) the etching waste liquid from an etching liquid outlet, and storing for preparing other production processes.
2. The apparatus for distilling and recovering hydrogen chloride from acidic etching waste liquid according to claim 1, wherein: and an exhaust port (16) is arranged on the tertiary absorption tower (17).
3. The apparatus for distilling and recovering hydrogen chloride from acidic etching waste liquid according to claim 1, wherein: stirring motor (4) are connected with stirring vane (37) through the transmission shaft, and stirring vane (37) are located inside reation kettle (1).
4. The apparatus for distilling and recovering hydrogen chloride from acidic etching waste liquid according to claim 1, wherein: all fixedly connected with shower (18) on condenser A (7), condenser B (11) and condenser C (15), each shower (18) end extends respectively to in primary absorption tower (8), secondary absorption tower (12) and the cubic absorption tower (17) tower.
5. The apparatus for distilling and recovering hydrogen chloride from acidic etching waste liquid according to claim 1, wherein: valves are arranged on the etching solution inlet (2), the etching solution outlet (38) and the pipeline A (5).
6. A distillation recovery method of hydrogen chloride in acidic etching waste liquid is characterized by comprising the following steps: the method comprises the following steps:
s1, feeding etching waste liquid with volume of 75% into a reaction kettle (1) along an etching liquid inlet (2), introducing heat conduction oil for heating, and keeping the temperature of the etching waste liquid in the reaction kettle within the range of 105-115 ℃; simultaneously, clear water with the volume of 1/3 is introduced into the absorption towers;
s2, starting a stirring motor (4) to carry out distillation stirring, and separating out a mixed gas containing hydrogen chloride gas and water vapor from the etching waste liquid;
s3, when the temperature of the mixed gas in the reaction kettle (1) reaches 45-50 ℃, opening a valve arranged on a pipeline A (5), allowing the mixed gas to enter a condenser A (7) and enter a primary absorption tower (8) along a spray pipe for absorption; residual gas separated out from the primary absorption tower (8) enters a secondary absorption tower (12) along a pipeline C (9) for absorption, and residual gas separated out from the secondary absorption tower (12) enters a tertiary absorption tower (17) along a pipeline E (13) for absorption;
s4, when the concentration of the hydrogen chloride in the hydrochloric acid solution in the primary absorption tower (8) reaches a preset standard, opening a valve a (35), and discharging the hydrochloric acid in the primary absorption tower (8) into a finished product tank along a hydrochloric acid liquid outlet (36); opening a valve f (27), a valve g (25), a valve c (32) and a valve B (32), pumping the hydrochloric acid solution in the secondary absorption tower (12) into the primary absorption tower (8) along a pipeline H (28) through a pump B (26); opening a valve I (22), a valve j (19) and a valve e (29), pumping the hydrochloric acid solution in the tertiary absorption tower (17) into the secondary absorption tower (12) along a pipeline I (20) through a pump C (21), and completing the rotation of the hydrochloric acid solution in the primary absorption tower (8) and the secondary absorption tower (12);
s5, after the hydrochloric acid in the tertiary absorption tower (17) is transferred, opening a valve h (24) on a clear water inlet (23) to introduce clear water into the tertiary absorption tower (18);
and S6, after the concentration of the hydrochloric acid in the etching waste liquid distilled in the reaction kettle is reduced to a preset standard, discharging (38) the etching waste liquid from an etching liquid outlet, and storing for other production processes.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104944665A (en) * | 2015-06-19 | 2015-09-30 | 浙江大学 | Comprehensive resourceful treatment device and method for chlorohydric acid pickling waste liquid |
| CN206652384U (en) * | 2017-04-20 | 2017-11-21 | 广东省博罗县湘澧精细化工有限公司 | Thtee-stage shiplock ammonia absorber |
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| US3469370A (en) * | 1968-05-31 | 1969-09-30 | Atlantic Richfield Co | Purification of hydrogen chloride produced during the alkylation of benzene with chloroparaffins |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104944665A (en) * | 2015-06-19 | 2015-09-30 | 浙江大学 | Comprehensive resourceful treatment device and method for chlorohydric acid pickling waste liquid |
| CN206652384U (en) * | 2017-04-20 | 2017-11-21 | 广东省博罗县湘澧精细化工有限公司 | Thtee-stage shiplock ammonia absorber |
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