CN109626330A - The distillation recovery device and method of hydrogen chloride in a kind of acidic etching waste liquid - Google Patents
The distillation recovery device and method of hydrogen chloride in a kind of acidic etching waste liquid Download PDFInfo
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- CN109626330A CN109626330A CN201910045614.4A CN201910045614A CN109626330A CN 109626330 A CN109626330 A CN 109626330A CN 201910045614 A CN201910045614 A CN 201910045614A CN 109626330 A CN109626330 A CN 109626330A
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- absorption tower
- pipeline
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- condenser
- hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
- ing And Chemical Polishing (AREA)
- Gas Separation By Absorption (AREA)
Abstract
The invention discloses a kind of distillation recovery devices of hydrogen chloride in acidic etching waste liquid, it includes reaction kettle (1) and circulation absorption system, and stirring motor (4), temperature detector (3), etching solution import (2) and etching solution outlet (38) are provided on the reaction kettle (1)；The circulation absorption system include an absorption tower (8), double absorption tower (12) and three times absorption tower (17) and an absorption tower (8), double absorption tower (12) and on absorption tower (17) be fixedly installed condenser A(7 respectively three times), condenser B(11) and condenser C(15)；It is provided with pump and valve on each absorption tower, the transfer for realizing acid solution is connected to be stepped up concentration of hydrochloric acid by pipeline between absorption tower；The invention has the following beneficial effects: low concentration of salt acid solution can be further diverted into other absorption towers to increase recovery efficiency, and cost recovery is low, does not add and generate new harmful substance using reaction kettle distillation and multistage recovery tower cyclic absorption.
Description
Technical field
The present invention relates to field of industrial waste water treatment, in particular to the distillation recovery of hydrogen chloride in a kind of acidic etching waste liquid
Device and method.
Background technique
Pcb board, which etches, is discharged a large amount of hydrochloric waste water in production line, according to conventional treatment, take off after need to being neutralized with alkali
Salt treatment not only consumes a large amount of alkali, while also generating a large amount of salt, and due to concentration of hydrochloric acid too it is low can not reuse, directly arrange
It puts and is unfavorable for environmental protection and save cost.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings of the existing technology, provides a kind of use distillation mode multiple stage circulation absorption,
It is at low cost, the recyclable device and recovery method of hydrogen chloride in the etching waste liquor without adding medicament.
The purpose of the present invention is achieved through the following technical solutions: the distillation recovery of hydrogen chloride in a kind of acidic etching waste liquid
Device, it includes reaction kettle and circulation absorption system that it, which includes it, be provided on the reaction kettle stirring motor, temperature detector,
Etching solution import and etching solution outlet；The circulation absorption system includes an absorption tower, double absorption tower and absorption tower three times,
Absorption tower, double absorption tower and condenser A, condenser B and condenser C are respectively arranged on absorption tower three times；It is described anti-
Kettle is answered to pass through absorption tower of pipeline B connection lower part by pipeline A connection condenser A, condenser A；Absorption tower is logical
Piping C is connected with condenser B；Condenser B passes through pipeline D connection double absorption tower lower part；The double absorption tower passes through pipe
Road E connection condenser C, condenser C pass through pipeline F connection absorption tower lower part three times.
Further, the reaction kettle is enamel reaction still, and reaction kettle inner heat source is provided by heat-conducting oil furnace.
Further, valve is provided on the etching solution import, etching solution outlet and pipeline A.
Further, it is provided with valve and pump on the pipeline B, pipeline D and pipeline F, is i.e. is provided with pump A on pipeline B
With valve b, it is provided on pipeline D on pump B and valve f, pipeline F and is provided with pump C and valve i.
Further, the absorption tower lower part is additionally provided with hydrochloric acid liquid outlet, is provided with valve on hydrochloric acid liquid outlet
a。
Further, the lower part of absorption tower three times is provided with clear water entrance, and valve h is provided on clear water entrance.
Further, the pipeline B is connected with pipeline G by threeway on one section between condenser A and pump A, manages
The road G other end connects sulfuric acid liquid outlet, is provided with valve d on pipeline G.
Further, the pipeline D is connected with pipeline H by threeway on one section between condenser B and pump B, manages
The road H other end is located between valve b and pump A on the pipeline B of section using threeway connection, and valve g is provided on pipeline H.
Further, the pipeline F is connected with pipeline I by threeway on one section between condenser C and pump C, manages
The road I other end connects double absorption tower bottom, is provided with valve j on pipeline I.
A kind of distillation recovery method of hydrogen chloride in acidic etching waste liquid, it is characterised in that: it the following steps are included:
S1. etching waste liquor is passed through in reaction kettle, is passed through heat-conducting oil heating and keeps in reaction kettle etching waste liquor temperature in 105-
Within the scope of 115 DEG C；The clear water of its volume 1/3 is passed through in each absorption tower simultaneously；
S2. it opens stirring motor and carries out distillation stirring, the mixed gas of gas containing hydrogen chloride and vapor is precipitated in etching waste liquor；
S3. when mixed gas temperature reaches 45-50 DEG C in reaction kettle, the valve being arranged on opening conduits A, mixed gas enters
Condenser A and along spray tube enter an absorption tower in absorbed；Residual gas is precipitated in absorption tower to enter along pipeline C
It is absorbed in double absorption tower, precipitation residual gas enters in absorption tower three times along pipeline E and absorbed in double absorption tower；
S4. it when hydrogen cloride concentration reaches preset standard in hydrochloric acid solution in an absorption tower, opens in the absorption tower valve a
Hydrochloric acid is discharged into pan tank along hydrochloric acid liquid outlet；Open valve f, valve g, valve c and valve b, double absorption Ta Neinei hydrochloric acid
Solution enters an absorption tower along pipeline H through pump B suction；Open valve i, valve j and valve e, hydrochloric acid is molten in absorption tower three times
Liquid is entered in double absorption tower by pump C suction along pipeline I, and the rotation of acid solution in an absorption tower and double absorption tower is completed；
S5. after the completion of hydrochloric acid transfer in absorption tower three times, the valve h on clear water entrance is opened, is passed through in absorption tower three times
Clear water；
S6. after the etching waste liquor concentration of hydrochloric acid after distilling in reaction kettle drops to preset standard, discharge is exported from etching solution and is excluded
And store, in case other production processes.
The invention has the following advantages that
Using physical method using reaction kettle distillation and multistage recovery tower cyclic absorption, low concentration of salt acid solution can be shifted further
To other absorption towers to increase recovery efficiency, cost recovery is low, does not add and generate new harmful substance.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention；
In figure: 1- reaction kettle, 2- etching solution import, 3- temperature detector, 4- stirring motor, 5- pipeline A, 6- pipeline B, 7- condensation
The absorption tower device A, 8-, 9- pipeline C, 10- pipeline D, 11- condenser B, 12- double absorption tower, 13- pipeline E, 14- pipeline F,
15- condenser C, 16- exhaust outlet, absorption tower, 18- spray tube, 19- valve j, 20- pipeline I, 21- pump C, 22- valve to 17- three times
I, 23- clear water entrance, 24- valve h, 25- valve g, 26- pump B, 27- valve f, 28- pipeline H, 29- valve e, 30- valve d,
31- pumps A, 32- valve c, 33- valve b, 34- pipeline G, 35- valve a, 36- hydrochloric acid liquid outlet, 37- stirring blade, 38- etching
Liquid outlet.
Specific embodiment
The present invention will be further described with reference to the accompanying drawing, but protection scope of the present invention is not limited to following institute
It states.
As shown in Figure 1, in a kind of acidic etching waste liquid hydrogen chloride distillation recovery device, it include reaction kettle 1 and circulation
Absorption system is provided with stirring motor 4, temperature detector 3, etching solution import 2 and etching solution outlet 38 on the reaction kettle 1,
The temperature detector 3 is equipped with two groups altogether, and one group is used to detect etching waste liquor temperature, and another group for detecting gas in reaction kettle 1
Temperature；The stirring motor 4 is connected with stirring blade 37 by transmission shaft, and stirring blade 37 is located inside reaction kettle 1.
The circulation absorption system includes an absorption tower 8, double absorption tower 12 and absorption tower 17 three times, wherein primary inhale
Receive tower 8, double absorption tower 12 and three times on absorption tower 17 installation settings has condenser A7, condenser B11 and condenser respectively
C15；Pipeline A5 is provided at the top of the reaction kettle 1, the pipeline A5 other end connects condenser A7, and condenser A7 is connected by pipeline B6
8 lower part of an absorption tower is connect, 8 lower part of an absorption tower is provided with hydrochloric acid liquid outlet 36, is provided on hydrochloric acid liquid outlet 36
Valve a35；It is provided with pump A31 and valve b33, pipeline B6 on the pipeline B6 and is being located between condenser A7 and pump A31 one section
Upper to be connected with pipeline G34 by threeway, pipeline G34 other end threeway connects hydrochloric acid liquid outlet 36, is provided with valve on pipeline G34
d30；Absorption tower 8 is connected by pipeline C9 with condenser B11, and condenser B11 passes through pipeline D10 connection double absorption
12 lower part of tower；Pump B26 and valve f27, pipeline D10 is provided on the pipeline D10 to be located between condenser B11 and pump B26
Pipeline H28 is also connected with by threeway on one section, the pipeline H28 other end is located between valve b33 and pump A31 using threeway connection
On the pipeline B6 of section, valve g25 and valve c32 are provided on pipeline H28；The double absorption tower 12 is connected by pipeline E13
Condenser C15, condenser C15 pass through pipeline F14 connection 17 lower part of absorption tower three times；Be provided on the pipeline F14 pump C21 and
Valve i22, pipeline F14 are connected with pipeline I20, pipeline I20 by threeway on one section between condenser C15 and pump C21
The other end connects 12 bottom of double absorption tower, is provided with valve j19 and valve e29 on pipeline I20；On the absorption tower three times 17
Portion is provided with exhaust outlet 16, and 17 lower part of absorption tower is provided with clear water entrance 23 three times, and valve h24 is provided on clear water entrance 23.
The reaction kettle 1 is enamel reaction still, and 1 inner heat source of reaction kettle is provided by heat-conducting oil furnace；The condenser A7, condensation
Spray tube 18 is fixedly connected on device B11 and condenser C15,18 end of spray tube extends to absorption tower 8, a double absorption
In tower 12 and three times 17 tower of absorption tower；Valve is provided on the etching solution import 2, etching solution outlet and 38 and pipeline A5
To control uninterrupted.
A kind of distillation recovery method of hydrogen chloride in acidic etching waste liquid, it is characterised in that: it the following steps are included:
S1. etching waste liquor is passed through in reaction kettle 1 along etching solution import 2, passes through heat-conducting oil heating and keeps etching in reaction kettle 1
Waste liquid temperature is within the scope of 105-115 DEG C；Open valve h24, valve i22, valve j19, valve e29, valve f27, valve simultaneously
Door g25, valve c32, valve b33, at pump C21, pump B26 and pump A31 work, clear water enters along clear water entrance 23 to be absorbed three times
In tower 17, and successively enter double absorption tower 12 along pipeline I20, enters an absorption tower 8 along pipeline H28, and respectively along pipeline
B6, pipeline D10 and pipeline the F14 circulated sprinkling between each absorbing tower bottom and tower top；Absorption tower 8, double absorption tower 12
Clear water amount is passed through in absorption tower 17 three times to be the 1/3 of own volume and flood 18 end of spray tube；When clear water is passed through end
Afterwards, valve described above is closed；
S2. it opens stirring motor 4 and carries out distillation stirring, the gaseous mixture of gas containing hydrogen chloride and vapor is precipitated in etching waste liquor
Body；
S3. when mixed gas temperature reaches 45-50 DEG C in reaction kettle, the valve being arranged on opening conduits A5, mixed gas into
Enter condenser A7, and enters in an absorption tower 8 along spray tube 18 and absorbed；Residual gas edge is precipitated in absorption tower 8
Pipeline C9 and condenser B11, which enters in double absorption tower 12, to be absorbed, and residual gas is precipitated in double absorption tower 12 along pipeline
E13 and condenser C15, which enter in absorption tower 17 three times, to be absorbed, the concentration of hydrochloric acid that absorbing hydrogen chloride is formed in each absorption tower according to
Secondary reduction, residual exhaust are discharged into other along exhaust outlet 16 and collect processing routine；
S4. when hydrogen cloride concentration reaches preset standard in hydrochloric acid solution in an absorption tower 8, valve a35 is opened, it is primary to absorb
Hydrochloric acid is discharged into pan tank along hydrochloric acid liquid outlet 35 in tower 8；Open valve f27, valve g25, valve c32 and valve b33, it is secondary
Hydrochloric acid solution enters in an absorption tower 8 through pump B26 suction along pipeline H28 in absorption tower 12；Open valve i22, valve j19 and
Valve e29, hydrochloric acid solution is entered in double absorption tower 12 by pump C21 suction along pipeline I20 in absorption tower 17 three times, completes one
The rotation of acid solution in secondary absorption tower 8 and double absorption tower 12；
S5. after the completion of hydrochloric acid transfer in absorption tower 17 three times, the valve h24 on clear water entrance 23 is opened, toward absorption tower three times
Clear water is passed through in 17；
S6. after the etching waste liquor concentration of hydrochloric acid after distilling in reaction kettle 1 drops to preset standard, from 38 discharge row of etching solution outlet
It removes and stores, in case other production processes.
Hydrochloric acid concentration in etching solution is different, and boiling temperature is not also identical when distilling, in the present embodiment, hydrochloric acid solution
Boiling point is 110 DEG C, reaches 25% or more using the concentration of hydrochloric acid solution generated after the present apparatus and method distillation, meets etching solution
The reuse concentration of required hydrochloric acid in regeneration.
Claims (14)
1. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid, it is characterised in that: it includes reaction kettle (1) and circulation
Absorption system is provided with stirring motor (4), temperature detector (3), etching solution import (2) and etching solution on the reaction kettle (1)
It exports (38)；The circulation absorption system includes an absorption tower (8), double absorption tower (12) and three times absorption tower (17) and one
Secondary absorption tower (8), double absorption tower (12) and on absorption tower (17) be fixedly installed condenser A(7 respectively three times), condenser B
(11) and condenser C(15)；The reaction kettle (1) passes through pipeline A(5) connection condenser A(7), condenser A(7) and pass through pipeline B
(6) absorption tower (8) lower part is connected；Absorption tower (8) passes through pipeline C(9) and condenser B(11) connection；Condensation
Device B(11) pass through pipeline D(10) connection double absorption tower (12) lower part；The double absorption tower (12) passes through pipeline E(13) even
Meet condenser C(15), condenser C(15) pass through pipeline F(14) connect absorption tower (17) lower part three times.
2. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that: institute
It states and is provided with exhaust outlet (16) on absorption tower (17) three times.
3. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that: institute
It states stirring motor (4) to be connected with stirring blade (37) by transmission shaft, stirring blade (37) is located at internal in reaction kettle (1).
4. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that: institute
State condenser A(7), condenser B(11) and condenser C(15) on be fixedly connected to spray tube (18), each spray tube (18) end
End extends respectively into an absorption tower (8), double absorption tower (12) and three times in absorption tower (17) tower.
5. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that: institute
State etching solution import (2), etching solution outlet (38) and pipeline A(5) on be provided with valve.
6. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that: institute
State pipeline B(6) on be provided with pump A(31) and valve b(33).
7. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that: institute
State pipeline D(10) on be provided with pump B(26) and valve f(27).
8. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that: institute
State pipeline F(14) on be provided with pump C(21) and valve i(22).
9. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that: institute
It states absorption tower (8) lower part to be provided with hydrochloric acid liquid outlet (36), hydrochloric acid liquid outlet is provided with valve a(35 on (36)).
10. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 1, it is characterised in that:
Absorption tower three times (17) lower part is provided with clear water entrance (23), and clear water entrance is provided with valve h(24 on (23)).
11. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 6, it is characterised in that:
The pipeline B(6) in condenser A(7) and pump A(31) between one section of upper threeway be connected with pipeline G(34), pipeline G(34) it is another
Hold threeway connection hydrochloric acid liquid outlet (36), pipeline G(34) on be provided with valve d(30).
12. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 7, it is characterised in that:
The pipeline D(10) be located at condenser B(11) and pump B(26) between pipeline H(28 is also connected with by threeway on one section), manage
Road H(28) other end using threeway connection be located at valve b(33) and pump A(31) between section pipeline B(6) on, pipeline H(28) on
It is provided with valve g(25) and valve c(32).
13. the distillation recovery device of hydrogen chloride in a kind of acidic etching waste liquid according to claim 8, it is characterised in that:
The pipeline F(14) be located at condenser C(15) and pump C(21) between one section go up pipeline I(20 is connected with by threeway), pipeline
I(20) other end connect double absorption tower (12) bottom, pipeline I(20) on be provided with valve j(19) and valve e(29).
14. a kind of distillation recovery method of hydrogen chloride in acidic etching waste liquid, it is characterised in that: it the following steps are included:
S1. the etching waste liquor for putting into its volume 75% toward reaction kettle (1) along etching solution entrance (2), is passed through heat-conducting oil heating and keeps
Etching waste liquor temperature is within the scope of 105-115 DEG C in reaction kettle；The clear water that its volume 1/3 is passed through in tower is received on each absorption tower simultaneously；
S2. stirring motor (4) are opened and carry out distillation stirring, the gaseous mixture of gas containing hydrogen chloride and vapor is precipitated in etching waste liquor
Body；
S3. when mixed gas temperature reaches 45-50 DEG C in reaction kettle (1), opening conduits A(5) on the valve that is arranged, gaseous mixture
Body enters condenser A(7) it carries out, and enter in an absorption tower (8) along spray tube and absorbed；Analysis in absorption tower (8)
Residual gas enters in double absorption tower (12) along pipeline C(9) and is absorbed out, and residual gas is precipitated in double absorption tower (12)
Enter in absorption tower (17) three times along pipeline E(13) and is absorbed；
S4. when hydrogen cloride concentration reaches preset standard in an interior hydrochloric acid solution of absorption tower (8), valve a(35 is opened), once
Absorption tower (8) interior hydrochloric acid is discharged into pan tank along hydrochloric acid liquid outlet (36)；Open valve f(27), valve g(25), valve c(32)
With valve b(32), (12) interior hydrochloric acid solution is through pumping B(26 in double absorption tower) suction along pipeline H(28) enters an absorption tower
(8)；Open valve i(22), valve j(19) and valve e(29), three times absorption tower (17) interior hydrochloric acid solution by pump C(21) take out
It inhales and enters in double absorption tower (12) along pipeline I(20), complete the wheel an of absorption tower (8) and double absorption tower (12) interior acid solution
It changes；
S5. after the completion of the transfer of absorption tower three times (17) interior hydrochloric acid, the valve h(24 on clear water entrance (23) is opened) toward inhaling three times
It receives in tower (18) and is passed through clear water；
S6. after the etching waste liquor concentration of hydrochloric acid after distilling in reaction kettle drops to preset standard, discharge (38) is exported from etching solution
It excludes and stores, in case other production processes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910045614.4A CN109626330B (en) | 2019-01-17 | 2019-01-17 | Distillation recovery device and method for hydrogen chloride in acidic etching waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910045614.4A CN109626330B (en) | 2019-01-17 | 2019-01-17 | Distillation recovery device and method for hydrogen chloride in acidic etching waste liquid |
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| Publication Number | Publication Date |
|---|---|
| CN109626330A true CN109626330A (en) | 2019-04-16 |
| CN109626330B CN109626330B (en) | 2022-11-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115991457A (en) * | 2023-02-24 | 2023-04-21 | 中国矿业大学 | Recovery device and recovery method for hydrochloric acid in chlorination distillation waste acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3469370A (en) * | 1968-05-31 | 1969-09-30 | Atlantic Richfield Co | Purification of hydrogen chloride produced during the alkylation of benzene with chloroparaffins |
| 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 |
-
2019
- 2019-01-17 CN CN201910045614.4A patent/CN109626330B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3469370A (en) * | 1968-05-31 | 1969-09-30 | Atlantic Richfield Co | Purification of hydrogen chloride produced during the alkylation of benzene with chloroparaffins |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115991457A (en) * | 2023-02-24 | 2023-04-21 | 中国矿业大学 | Recovery device and recovery method for hydrochloric acid in chlorination distillation waste acid |
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