CN108525337A - A kind of dilute hydrochloric acid is concentrated in vacuo tower and its application method - Google Patents
A kind of dilute hydrochloric acid is concentrated in vacuo tower and its application method Download PDFInfo
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- CN108525337A CN108525337A CN201810530336.7A CN201810530336A CN108525337A CN 108525337 A CN108525337 A CN 108525337A CN 201810530336 A CN201810530336 A CN 201810530336A CN 108525337 A CN108525337 A CN 108525337A
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- hydrochloric acid
- tower
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Treating Waste Gases (AREA)
Abstract
The present invention relates to a kind of dilute hydrochloric acid to be concentrated in vacuo tower and its application method, include sequentially from bottom to top hydrochloric acid explosive evaporation section, dilute hydrochloric acid stripping dehydration enriching section and return of waste water absorbing hydrogen chloride section, reboiler boiling mixed in hydrochloric acid import is equipped at the top of hydrochloric acid explosive evaporation section, bottom is exported equipped with concentrate acid;It is equipped with dilute hydrochloric acid import at the top of dilute hydrochloric acid stripping dehydration enriching section, the first low sprinkle density liquid distribution trough, the first packing layer are sequentially equipped with below dilute hydrochloric acid import;It is equipped with return of waste water import at the top of return of waste water absorbing hydrogen chloride section, the second low sprinkle density liquid distribution trough, the second packing layer are sequentially equipped with below return of waste water import.22% or more is concentrated into after dilute hydrochloric acid is processed by the invention, while hydrogen chloride content is not more than 1% in overhead vapor stream;Due to be concentrated in vacuo tower in do not add calcium chloride or other, so there is no fouling and block the problems such as;The present invention has many advantages, such as that reliability is high, resistance to pressure is good, it is strong, easy for installation to adapt to failures.
Description
Technical field
The present invention relates to a kind of enrichment facilities, and tower and its application method are concentrated in vacuo more particularly, to a kind of dilute hydrochloric acid.
Background technology
By the end of about 23,000,000 tons/year of domestic PVC total productive capacity of in December, 2017, wherein former using calcium carbide
Material process route device accounts for about 83%, remaining is ethylene subtraction unit.In carbide raw material route process units, VCM is purified back
Due to containing mercury element (mercury chloride is the catalyst for being converted into VCM) in the hydrochloric acid of receipts, cannot discharge, therefore VCM is purified back
The hydrochloric acid of receipts has been all made of resolving hydrochloric acid technology, and recycling hydrogen chloride recycles, most in order to solve the problems, such as water balance
Resolving hydrochloric acid device is divided into two parts:The deep analysis (Calcium Chloride Method) of the conventional resolution of concentrated hydrochloric acid+part dilute hydrochloric acid, calcium chloride
The water that method complete solution analysis part mainly parses Low acid (~1%HCL) returns to purification combination water scrubber.Currently running chlorination
There are following disadvantages in commercial practice for the full analysis unit of calcium method dilute hydrochloric acid:
(1), it since Calcium Chloride Method dilute hydrochloric acid complete solution analysis apparatus technological temperature is high (120 DEG C~135 DEG C of bottom temperature), then boils
High (≤the 0.6MPa of steam pressure (G) that device uses), cause the plant failure rate high, especially graphite reboiler.
(2), due to high calcium chloride concentration aqueous solution the characteristics of, it is easy the fouling at reboiler hole wall, leads to its heat transfer effect
Rate declines, and eventually leads to reboiler cisco unity malfunction.
So in actual industrialization operation, blocks in order to prevent, improve the cycle of operation of device, current enterprise uses
The method of calcium chloride salt acid solution in regular displacement apparatus, prevents harmful ion from accumulating.Typical method is Calcium Chloride Method depth
Calcium chloride is primary in resolver first quarter exchange system, and year replaces 4 times or so.The drawbacks of doing so, which is device, must discharge and contain
The dilute waste solution of calcium chloride of mercury, device do not accomplish real " zero " discharge.And the mercurous dilute waste solution of calcium chloride amount always discharged in year is not
Few, by taking typical 300,000 tons of PVC devices as an example, annual emissions reach 20~25 tons of mercurous dilute waste solution of calcium chloride.It is mercurous with high salt
Waste liquid needs high processing cost.
Invention content
In order to overcome the shortcomings of the prior art, the present invention provides a kind of dilute hydrochloric acid to be concentrated in vacuo tower and its user
Method.
A kind of dilute hydrochloric acid is concentrated in vacuo tower, and the vacuums concentration tower is from bottom to top sequentially including hydrochloric acid explosive evaporation section, dilute
Hydrochloric acid stripping dehydration enriching section and return of waste water absorbing hydrogen chloride section, the hydrochloric acid explosive evaporation section top are equipped with reboiler and boil
Mixed in hydrochloric acid import, hydrochloric acid explosive evaporation section bottom are exported equipped with concentrate acid;It is set at the top of the dilute hydrochloric acid stripping dehydration enriching section
There is dilute hydrochloric acid import, the first low sprinkle density liquid distribution trough is equipped with below the dilute hydrochloric acid import, the first low spray is close
It spends and is equipped with the first packing layer below liquid distribution trough;Return of waste water import is equipped at the top of the return of waste water absorbing hydrogen chloride section,
The second low sprinkle density liquid distribution trough, the second low sprinkle density liquid distribution trough are equipped with below the return of waste water import
Lower section is equipped with the second packing layer.
Preferably, first packing layer, the second packing layer are non-metallic plates corrugated filler layer.
Preferably, the vacuum concentration top of tower is equipped with steam outlet, it is equipped with and removes above the return of waste water import
Day with fog component.
Preferably, the hydrochloric acid explosive evaporation section, dilute hydrochloric acid stripping dehydration enriching section and return of waste water absorbing hydrogen chloride
Section is equipped with corresponding manhole.
Preferably, the hydrochloric acid explosive evaporation section bottom is equipped with thermometer mouth and first liquid level gauge mouth, the hydrochloric acid boiling
It rises and is equipped with second liquid level gauge mouth in the middle part of evaporator section, pressure gauge port is equipped with above the reboiler boiling mixed in hydrochloric acid import.
Preferably, the dilute hydrochloric acid import, the outlet of concentrate acid are connected with concentrated hydrochloric acid Analytic Tower respectively.
Preferably, the vacuum concentration tower outer wall is equipped with the outer stiffening ring of tower body.
A kind of dilute hydrochloric acid is concentrated in vacuo the application method of tower, includes the following steps:
(1) entered by dilute hydrochloric acid import after the dilute hydrochloric acid metering from concentrated hydrochloric acid Analytic Tower and be concentrated in vacuo in tower, the
It is mixed with from the diluted acid water phegma for being concentrated in vacuo tower epimere on one low sprinkle density liquid distribution trough, it is then low by first
Sprinkle density liquid distribution trough is uniformly distributed in the first packing layer, with through reboiler heating vaporization hydrogen chloride and water vapour it is close
Cut-grafting is touched, and under the conditions of certain vacuum degree, relatively low-boiling water vapour part is stripped out dilute hydrochloric acid solution, with mixed vapour
Rise to the return of waste water absorbing hydrogen chloride section for being concentrated in vacuo tower;
(2) above-mentioned mixed vapour is returned with after the outer steam condenser condensation of vacuum concentration tower by return of waste water import
It flow to the acid waste water close contact for being concentrated in vacuo tower top, extra hydrogen chloride gas, which is absorbed, in mixed vapour returns to vacuum
Concentration tower, the water vapour and a small amount of hydrogen chloride for meeting process goal evaporate vacuum concentration tower by steam outlet;
(3) the concentrate hydrochloric acid being concentrated in vacuo in tower returns to the cycle parsing of concentrated hydrochloric acid Analytic Tower by liquid automatic control.
The operation principle of the present invention:
Using the different physical property design of azeotrope composition concentration of dilute hydrochloric acid at various pressures, such as in normal pressure
The composition of lower azeotropic dilute hydrochloric acid is hydrogen chloride 20.24% and water 79.76%;When pressure reduction is to 30KPaA, azeotropic dilute hydrochloric acid
Composition be hydrogen chloride 22.5% and water 77.5%.In this way to the barostat control parsed with normal pressure, stripped by heating under reduced pressure
Part water can be isolated, to concentrate dilute hydrochloric acid.
The present invention is due to the deep-etching characteristic of hydrochloric acid, and tower body and the distribution of tower internals material are using different highly corrosion resistants, height
Intensity nonmetallic materials such as fiberglass or PPH manufactures, have better mechanical performance compared with common graphite resolving hydrochloric acid tower,
Reliability, high pressure;It is strong to adapt to failures;Whole tower light weight, shock resistance is good, easy for installation;Solving reliability
While problem, economy has been taken into account.
Preferably, mass concentration >=22% of concentrate hydrochloric acid, hydrogen chloride content is not more than 1% in overhead vapor stream.
Preferably, the first low sprinkle density liquid distribution trough, the second low sprinkle density liquid distribution trough use phenol
Aldehyde epoxy vingl ester resin base glass steel material is fabricated.Intensity is high, and hydrochloric acid corrosion resistant performance is good, good reliability.
For existing polyvinyl chloride factory VCM purification resolving hydrochloric acid device there are the problem of:Dilute hydrochloric acid Calcium Chloride Method complete solution
Analysis apparatus high failure rate, the cycle of operation are short;There is mercurous dilute waste solution of calcium chloride discharge;And the spy of VCM purification resolving hydrochloric acid devices
Point, we are concentrated in vacuo subsystem using dilute hydrochloric acid and replace Calcium Chloride Method dilute hydrochloric acid complete solution analysis subsystem, under certain vacuum degree
Change dilute hydrochloric acid azeotropic concentration composition, the water for isolating part Low acid (~1%HCL) returns to purification combination water scrubber, solves
The water balance of whole device.The advantages of designing in this way is the calcium chloride solution for not having easy fouling in system, and system is not mercurous
Dilute waste solution of calcium chloride discharge.Dilute hydrochloric acid is concentrated in vacuo subsystem and is run under certain vacuum degree simultaneously, and dilute hydrochloric acid boiling temperature is low,
The heating steam pressure needed is low, solves the integrity problem of device, meets new process device long period continuous operation
It is required that.The dilute hydrochloric acid of the present invention is concentrated in vacuo the core equipment that tower is above-mentioned new process, it is permanent according to dilute hydrochloric acid under different pressures
Boiling object forms different principle exploitations, while also solving the technique that heat and quality under low sprinkle density effectively transmit
Problem.
The beneficial effects of the present invention are:
(1) it is concentrated in vacuo tower dilute hydrochloric acid through the invention and is concentrated into 22% or more, while hydrogen chloride in overhead vapor stream
Content is not more than 1%;
(2) due to be concentrated in vacuo tower in do not add calcium chloride or other, so there is no fouling and block the problems such as;
(3) present invention has many advantages, such as that reliability is high, resistance to pressure is good, it is strong, easy for installation to adapt to failures.
Description of the drawings
Fig. 1 is the structural diagram of the present invention.
Specific implementation mode
The invention will be further described in the following with reference to the drawings and specific embodiments, but invention which is intended to be protected is simultaneously
It is without being limited thereto.
Referring to Fig.1, a kind of dilute hydrochloric acid is concentrated in vacuo tower, and the vacuum concentration tower includes sequentially from bottom to top that hydrochloric acid boiling is steamed
Section 1, dilute hydrochloric acid stripping dehydration enriching section 2 and return of waste water absorbing hydrogen chloride section 3 are sent out, 1 top of the hydrochloric acid explosive evaporation section is set
There is reboiler boiling mixed in hydrochloric acid import 4,1 bottom of hydrochloric acid explosive evaporation section is equipped with concentrate acid and exports 5;The dilute hydrochloric acid stripping is de-
2 top of water enriching section is equipped with dilute hydrochloric acid import 6, and 6 lower section of the dilute hydrochloric acid import is equipped with the first low sprinkle density liquid distribution trough
7, the first low sprinkle density liquid distribution trough, 7 lower section is equipped with the first non-metallic plates corrugated filler layer 8;The waste water returns
It flows 3 top of absorbing hydrogen chloride section and is equipped with return of waste water import 9,9 lower section of the return of waste water import is equipped with the second low sprinkle density
Liquid distribution trough 10, the second low sprinkle density liquid distribution trough, 10 lower section are equipped with the second non-metallic plates corrugated filler layer
11。
The vacuum concentration top of tower is equipped with steam outlet 12, and 9 top of the return of waste water import is equipped with demister group
Part 13.The hydrochloric acid explosive evaporation section, dilute hydrochloric acid stripping dehydration enriching section and return of waste water absorbing hydrogen chloride section are equipped with accordingly
Manhole 14.1 bottom of hydrochloric acid explosive evaporation section is equipped with thermometer mouth 15 and first liquid level gauge mouth 16, and the hydrochloric acid boiling is steamed
It sends out 1 middle part of section and is equipped with second liquid level gauge mouth 17,4 top of reboiler boiling mixed in hydrochloric acid import is equipped with pressure gauge port 18.Institute
State dilute hydrochloric acid import 6, concentrate acid outlet 5 is connected with concentrated hydrochloric acid Analytic Tower respectively.The vacuum concentration tower outer wall is equipped with tower
External stiffening ring 19.
Above-mentioned dilute hydrochloric acid is concentrated in vacuo the application method of tower, includes the following steps:
(1) entered by dilute hydrochloric acid import 6 after the dilute hydrochloric acid metering from concentrated hydrochloric acid Analytic Tower 19~20% and be concentrated in vacuo
In tower, mixed with from the diluted acid water phegma for being concentrated in vacuo tower epimere on the first low sprinkle density liquid distribution trough 7, then
It is uniformly distributed in the first packing layer 8 by the first low sprinkle density liquid distribution trough 7, with the chlorination through reboiler heating vaporization
Hydrogen and water vapour (are entered) close contact, under the conditions of certain vacuum degree, opposite low boiling by reboiler boiling mixed in hydrochloric acid import 4
The water vapour part of point is stripped out dilute hydrochloric acid solution, and the return of waste water absorption chlorination for being concentrated in vacuo tower is risen to mixed vapour
Hydrogen section;
(2) above-mentioned mixed vapour passes through return of waste water import 9 with after being concentrated in vacuo the outer steam condenser condensation of tower
Be back to the acid waste water close contact for being concentrated in vacuo tower top, in mixed vapour extra hydrogen chloride gas absorbed return it is true
Empty concentration tower, the water vapour and a small amount of hydrogen chloride for meeting process goal evaporate vacuum concentration tower by steam outlet 12;
(3) the concentrate hydrochloric acid being concentrated in vacuo in tower returns to the cycle parsing of concentrated hydrochloric acid Analytic Tower by liquid automatic control.
The operating temperature that the present invention is concentrated in vacuo tower is 70~80 DEG C, and operating pressure is -0.08MPa.
Tower body of the present invention is using highly corrosion resistant, high strength nonmetallic material such as fiberglass or PPH manufactures, with common graphite system
Resolving hydrochloric acid tower, which is compared, has better mechanical performance, reliability, high pressure;It is strong to adapt to failures;Whole tower light weight, anti-impact
It is good to hit performance, it is easy for installation.Low sprinkle density liquid distribution trough is manufactured using epoxy novolac vinylite base glass steel material,
Intensity is high, and hydrochloric acid corrosion resistant performance is good, good reliability.
The present invention is concentrated in vacuo tower and is broadly divided into three functional areas, is from bottom to top hydrochloric acid explosive evaporation section, dilute salt respectively
Acid stripping dehydration enriching section and return of waste water absorbing hydrogen chloride section;As long as dilute hydrochloric acid concentration meets≤22%, can be by this
Tower is concentrated into 22% or more, while hydrogen chloride content is not more than 1% in overhead vapor stream.The present invention and calcium chloride concentration tower ratio,
Do not added in the tower calcium chloride or other, so non flouling behaviour and blocking.
Claims (10)
1. a kind of dilute hydrochloric acid is concentrated in vacuo tower, it is characterised in that:The vacuum concentration tower includes sequentially from bottom to top that hydrochloric acid boils
Evaporator section, dilute hydrochloric acid stripping dehydration enriching section and return of waste water absorbing hydrogen chloride section, the hydrochloric acid explosive evaporation section top are equipped with
Reboiler boiling mixed in hydrochloric acid import, hydrochloric acid explosive evaporation section bottom is exported equipped with concentrate acid;The dilute hydrochloric acid stripping dehydration is dense
It is equipped with dilute hydrochloric acid import at the top of contracting section, is equipped with the first low sprinkle density liquid distribution trough below the dilute hydrochloric acid import, described the
It is equipped with the first packing layer below one low sprinkle density liquid distribution trough;Waste water is equipped at the top of the return of waste water absorbing hydrogen chloride section
Flow back import, and the second low sprinkle density liquid distribution trough, the second low sprinkle density are equipped with below the return of waste water import
The second packing layer is equipped with below liquid distribution trough.
2. dilute hydrochloric acid according to claim 1 is concentrated in vacuo tower, it is characterised in that:First packing layer, the second filler
Layer is non-metallic plates corrugated filler layer.
3. dilute hydrochloric acid according to claim 1 is concentrated in vacuo tower, it is characterised in that:The vacuum concentration top of tower is equipped with water
Steam (vapor) outlet, the return of waste water import top are equipped with demisting device assembly.
4. dilute hydrochloric acid according to claim 1 is concentrated in vacuo tower, it is characterised in that:The hydrochloric acid explosive evaporation section, dilute salt
Acid stripping dehydration enriching section and return of waste water absorbing hydrogen chloride section are equipped with corresponding manhole.
5. dilute hydrochloric acid according to claim 1 is concentrated in vacuo tower, it is characterised in that:The hydrochloric acid explosive evaporation section bottom is set
There are thermometer mouth and first liquid level gauge mouth, second liquid level gauge mouth, the reboiler boiling are equipped in the middle part of the hydrochloric acid explosive evaporation section
It rises and is equipped with pressure gauge port above mixed in hydrochloric acid import.
6. dilute hydrochloric acid according to claim 1 is concentrated in vacuo tower, it is characterised in that:The dilute hydrochloric acid import, concentrate acid go out
Mouth is connected with concentrated hydrochloric acid Analytic Tower respectively.
7. dilute hydrochloric acid according to claim 1 is concentrated in vacuo tower, it is characterised in that:The vacuum concentration tower outer wall is equipped with
The outer stiffening ring of tower body.
8. dilute hydrochloric acid described in a kind of claim 1 is concentrated in vacuo the application method of tower, it is characterised in that include the following steps:
(1) entered by dilute hydrochloric acid import after the dilute hydrochloric acid metering from concentrated hydrochloric acid Analytic Tower and be concentrated in vacuo in tower, it is low first
It is mixed with from the diluted acid water phegma for being concentrated in vacuo tower epimere on sprinkle density liquid distribution trough, then passes through the first low spray
Density fluid distributor is uniformly distributed in the first packing layer, is connect closely with the hydrogen chloride and water vapour vaporized through reboiler heating
It touches, under the conditions of certain vacuum degree, relatively low-boiling water vapour part is stripped out dilute hydrochloric acid solution, rises with mixed vapour
To the return of waste water absorbing hydrogen chloride section for being concentrated in vacuo tower;
(2) above-mentioned mixed vapour with from being concentrated in vacuo after the outer steam condenser condensation of tower through return of waste water circumfluence extremely
It is concentrated in vacuo the acid waste water close contact on tower top, extra hydrogen chloride gas, which is absorbed to return, in mixed vapour is concentrated in vacuo
Tower, the water vapour and a small amount of hydrogen chloride for meeting process goal evaporate vacuum concentration tower by steam outlet;
(3) the concentrate hydrochloric acid being concentrated in vacuo in tower returns to the cycle parsing of concentrated hydrochloric acid Analytic Tower by liquid automatic control.
9. dilute hydrochloric acid is concentrated in vacuo the application method of tower according to claim 8, it is characterised in that:The quality of concentrate hydrochloric acid is dense
>=22% is spent, hydrogen chloride content is not more than 1% in overhead vapor stream.
10. dilute hydrochloric acid is concentrated in vacuo the application method of tower according to claim 8, it is characterised in that:The first low spray
Density fluid distributor, the second low sprinkle density liquid distribution trough are manufactured using epoxy novolac vinylite base glass steel material
It forms.
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CN109503312A (en) * | 2019-01-15 | 2019-03-22 | 浙江迪邦化工有限公司 | A kind of technique of the by-product hydrogen chloride continuous production chloroethanes using chlorobenzene production |
CN111777041A (en) * | 2020-08-26 | 2020-10-16 | 伊犁南岗化工有限责任公司 | Deep analytical equipment of olefine acid concentration |
CN113023677A (en) * | 2021-02-26 | 2021-06-25 | 南通星球石墨股份有限公司 | Hydrochloric acid defluorination process system |
CN113041772A (en) * | 2021-03-30 | 2021-06-29 | 夏县运力化工有限公司 | Novel dilute hydrochloric acid rectifying tower |
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