CN110436505A - A kind of method of desulfurization co-production gypsum and calcium chloride - Google Patents
A kind of method of desulfurization co-production gypsum and calcium chloride Download PDFInfo
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- CN110436505A CN110436505A CN201910729421.0A CN201910729421A CN110436505A CN 110436505 A CN110436505 A CN 110436505A CN 201910729421 A CN201910729421 A CN 201910729421A CN 110436505 A CN110436505 A CN 110436505A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
- B01D53/501—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
- B01D53/502—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound characterised by a specific solution or suspension
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/96—Regeneration, reactivation or recycling of reactants
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/28—Chlorides by chlorination of alkaline-earth metal compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/32—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/40—Alkaline earth metal or magnesium compounds
- B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/60—Inorganic bases or salts
- B01D2251/604—Hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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Abstract
The present invention provides the methods of a kind of desulfurization co-production gypsum and calcium chloride, the method obtains the solution containing calcium chloride and calcium hydroxide after water logging goes out with epoxy propane saponified slag, calcium chloride concentration and pH value are controlled as desulfurization absorbing liquid, through aerating oxidation, and controls pH and obtain gypsum and calcium chloride.The method of the present invention is a kind of new using epoxy propane saponified slag as the method for desulfurizing agent co-production gypsum and calcium chloride, realize the comprehensive utilization of epoxy propane saponified slag, turn waste into wealth, saponification slag environmental pollution is reduced, and the mixing of calcium chloride and calcium hydroxide promotes the absorption of sulfur dioxide in the leachate of epoxy propane saponified slag.
Description
Technical field
The invention belongs to technical field of resource utilization, and in particular to a kind of method of desulfurization co-production gypsum and calcium chloride.
Background technique
China's propylene oxide is about 60% using the ratio of chlorohydrination production, which produces about 2,400,000 tons of propylene oxide often
Year, propylene oxide unit carbide slurry (or milk of lime) makees saponification agent, and the residue after saponification is epoxy propane saponified slag, production 1
Ton propylene oxide about generates 1-2 tons of saponification slags, and about 3,600,000 tons/year of discharge amount.
Currently, the comprehensive utilization of saponification slag mainly produces construction material, a kind of deicing salt (saponification slag preparation snow melt suppression ice
The method (CN201710341829.1) of functional material and the raw material as Soft Soil etc..By market and technical restriction, saponification slag
Still there are a large amount of stockpilings, generates many environmental problems.
Summary of the invention
There is provided it is an object of the invention to overcome in place of the shortcomings of the prior art a kind of desulfurization co-production gypsum and
The method of calcium chloride.
To achieve the above object, the technical scheme adopted by the invention is as follows: a kind of side of desulfurization co-production gypsum and calcium chloride
Method the described method comprises the following steps:
(1) epoxy propane saponified slag water logging is gone out, is separated by solid-liquid separation after leaching and obtains including calcium hydroxide and calcium chloride
Leachate A；
(2) the calcium chloride mass concentration in leachate A is controlled as 25%-35%, and is by the control of the pH value of leachate A
5.3-6.5, then using the leachate A for controlling calcium chloride concentration and pH as desulfurization absorbing liquid input in desulfuration absorbing tower with dioxy
Change sulphur to be mixed to obtain mixed liquid B；
(3) pH value for controlling mixed liquid B is 4.0-5.0 and aeration obtains mixture C into mixed liquid B, the aeration
It include oxygen in gas；
(4) filtered fluid D and solid E are obtained after being separated by solid-liquid separation mixture C, will obtain gypsum after solid E drying；
(5) mixed liquor F is obtained after mixing filtered fluid D with leachate A, and mixed liquor F is allocated as part A and part B, the portion A
Sub-control calcium chloride mass concentration is 25%-35%, pH value is 5.3-6.5 de- as the desulfurization absorbing liquid input in step (2)
In sulphur absorption tower, calcium chloride solution is prepared after the part B removal impurity of mixed liquor F, step evaporation of going forward side by side crystallizes to obtain calcium chloride.
The method of the present invention goes out to be separated by solid-liquid separation with the water logging of epoxy propane saponified slag, and obtaining main component is calcium chloride and hydrogen-oxygen
Change the leachate of calcium, leachate is as SO2Absorbing liquid inputs desulfurization in desulfurization equipment, then passes through aerating oxidation, is separated by solid-liquid separation
Solid product gypsum is obtained, filtered filtrate is sent into buffer pool, and mixed liquor a part circulation is used as SO2Absorbing liquid, a part
PH precipitating filtering removal impurity is adjusted, hydrochloric acid prepares calcium chloride after neutralizing.It is mainly that calcium chloride and calcium hydroxide are molten in leaching liquor
Liquid absorbs SO2Ability is strong, improves that desulfuration efficiency, liquid-gas ratio are low, and energy consumption reduces and prevents the scale problems in sweetening process.
The method of the present invention realizes the reasonable utilization of epoxy propane saponified slag, has effectively saved resource, has protected environment.
The chemical reaction that the method for the present invention step (2) and step (3) are related to is as follows:
Ca(OH)2+SO2=CaSO3↓+H2O
2CaSO3+O2=2CaSO4↓
2Ca(OH)2+2SO2+O2=2CaSO4↓+2H2O
CaSO3+SO2+H2O=Ca (HSO3)2
Ca(HSO3)2+O2=CaSO4↓+H2SO4
Preferably, in the step (5), the method for calcium chloride solution is prepared after the part B removal impurity of mixed liquor F are as follows:
The pH value of the part B of mixed liquor F is adjusted as 8.5-10, is with the pH that hydrochloric acid adjusts filtrate after separation of solid and liquid removal solid impurity
6.5-7.5 obtains calcium chloride solution.
The pH value for adjusting the part B of mixed liquor F is 8.5-10, can remove after separation of solid and liquid impurity magnesium in mixed liquor from
Son, aluminium ion, iron ion obtain the higher calcium chloride of purity, use salt acid for adjusting pH after separation of solid and liquid, convert calcium hydroxide to
Calcium chloride.
Preferably, in the step (2), the calcium chloride mass concentration in leachate A is controlled as 25%-35%.
Desulfurization when the calcium chloride mass concentration control in leachate A is 29%-31%, as sulphur dioxide absorbent
It is more efficient.
It preferably, is 6 by the pH value control in leaching liquor A in the step (2).
Preferably, in the step (3), the pH value for controlling mixed liquid B is 4.5.
Preferably, the step (3) carries out in aeration tank or aeration tower.
Preferably, in the step (2), the ratio of desulfurization absorbing liquid and sulfur dioxide is 0.5-8L/m3。
Preferably, in the step (2), the ratio of desulfurization absorbing liquid and sulfur dioxide is 2.0L/m3。
Preferably, the chemical composition of epoxy propane saponified slag are as follows: epoxy propane saponified cinder ladle includes the ingredient of following parts by weight:
Vector 20%-30%, calcium oxide 20%-65%, calcium chloride 1.57%-10.96% and impurity are burnt, institute's impurity includes that calorize is closed
Object, magnesium compound, iron compound and silicon compound.
Preferably, the pH adjusting agent in the step (2), in step (3) for controlling pH is acidic ph modifier, described
Acidic ph modifier is hydrochloric acid.
Preferably, in the step (5), the pH adjusting agent of the pH value of the part B of mixed liquor F is adjusted as alkaline pH adjusting
Agent, the alkaline pH adjusting agent are the leachate A of calcium hydroxide or saponification slag.
Preferably, in the step (3), the gas of aeration is air.
The beneficial effects of the present invention are: the present invention provides the methods of a kind of desulfurization co-production gypsum and calcium chloride, are
A method of it is new using epoxy propane saponified slag as desulfurizing agent co-production gypsum and calcium chloride, realize propylene oxide soap
Slugging comprehensive utilization, turns waste into wealth, and reduces calcium chloride in saponification slag environmental pollution and the leaching liquor of epoxy propane saponified slag
The absorption of sulfur dioxide is promoted with the mixing of calcium hydroxide.
Detailed description of the invention
Fig. 1 is the flow diagram of present invention method.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Embodiment 1
The method of a kind of desulfurization co-production gypsum and calcium chloride as the embodiment of the present invention, the method includes following steps
It is rapid:
(1) epoxy propane saponified slag water logging is gone out, is separated by solid-liquid separation after leaching and obtains including calcium hydroxide and calcium chloride
Leachate A；
(2) leachate A is inputted in buffer pool and is 31% and by adding by calcium chloride mass concentration control in leachate A
Adding hydrochloric acid to control the pH value of leachate A is 6.0, is then inhaled the leaching liquor A of calcium chloride concentration 31% and pH6.0 as desulfurization
It receives and is mixed in liquid input desulfuration absorbing tower with sulfur dioxide, desulfurization simultaneously obtains mixed liquid B, desulfurization absorbing liquid and sulfur dioxide
Ratio be 2.0L/m3；
(3) mixed liquor is inputted in aeration tank or aeration tower, controls the pH value 4.5 of mixed liquid B, and into mixed liquid B
Aeration obtains mixture C, and the gas of the aeration is air；
(4) filtered fluid D and solid E are obtained after being separated by solid-liquid separation mixture C, will obtain gypsum after solid E drying；
(5) mixed liquor F is obtained after mixing filtered fluid D with leachate A, mixed liquor F points are part A and part B, wherein A
Part control calcium chloride mass concentration is 31%, is 6.0 by addition hydrochloric acid control pH value as the desulfurization absorption in step (2)
Liquid inputs in desulfuration absorbing tower, and the part B of mixed liquor F adjusts pH value by the way that the leachate A of calcium hydroxide or saponification slag is added
For 8.5-10, after being separated by solid-liquid separation removal impurity, filtrate salt acid for adjusting pH value obtains calcium chloride solution for 7.0, and further steams
Hair crystallization obtains calcium chloride.
Leachate A includes calcium hydroxide and calcium chloride, and after reacting in desulfuration absorbing tower with sulfur dioxide, what is obtained is mixed
Closing in liquid B includes calcium sulfite, calcium bisulfite, calcium sulfate and calcium chloride, mixed liquid B sulfurous acid after air aeration
Calcium, calcium bisulfite are oxidized to calcium sulfate and calcium bisulfite and are completely converted into calcium sulfate by controlling pH value, i.e. in mixed liquor C
It include calcium sulfate and calcium chloride, calcium sulfate and calcium chloride separation, obtain gypsum and calcium chloride after purification after separation of solid and liquid
Product.
Embodiment 2
The method of a kind of desulfurization co-production gypsum and calcium chloride as the embodiment of the present invention, the present embodiment and embodiment 1
Method are as follows: in step (2), by leachate A calcium chloride mass concentration control be 30%.
Embodiment 3
The method of a kind of desulfurization co-production gypsum and calcium chloride as the embodiment of the present invention, the present embodiment and embodiment 1
Method are as follows: in step (2), by leaching liquor A calcium chloride mass concentration control be 25%.
Embodiment 4
The method of a kind of desulfurization co-production gypsum and calcium chloride as the embodiment of the present invention, the present embodiment and embodiment 1
Method are as follows: in step (2), by leaching liquor A calcium chloride mass concentration control be 35%.
Application examples 1
Using the method for embodiment 1 be as apply, it is specific as follows:
By taking 10t/h coal-burning boiler as an example, 130-140 DEG C of Initial Entry flue-gas temperature, inlet flue gas amount is 15332Nm3/ h,
Smoke inlet SO2Mean concentration is 991mg/Nm3, using flue gas bag collection+wet type desulfurizing technique.
A certain amount of epoxy propane saponified slag is taken, with water by counterflow leaching twice, is separated by solid-liquid separation, removal contains aluminium, iron, silicon
With the solid contents such as magnesium, the leachate A containing calcium hydroxide and calcium chloride is obtained, leachate A is inputted into buffer pool, controls calcium chloride
Concentration is 31%, and the pH of absorbing liquid A is 6.0 as desulfurization absorbing liquid；
Absorbing liquid is input in absorption tower by circulating pump, flue gas is passed in tower, liquid-gas ratio control exists in spray column
2.0L/m3, the calcium hydroxide in absorbing liquid reacts with the sulfur dioxide in flue gas Jing Guo dedusting, generates calcium sulfite, sulfurous acid
Hydrogen calcium and calcium sulfate；
It is inputted in oxidation and aeration pond after desulfurization absorbing liquid sulfur dioxide absorption by circulating pump, is adjusted with hydrochloric acid solution
PH is 4.5, and calcium sulfite, calcium bisulfite are oxidized to calcium sulfate at this time, is separated by solid-liquid separation, solid is dried to obtain gypsum, filtrate
Input buffer pool is mixed with leachate, is controlled calcium chloride concentration and pH value, is recycled as desulfurization absorbing liquid；
By the mixed liquor of filtrate and leachate in buffer pool, it is 8.5- that a part of mixed liquor, which is exported, and adjusts pH value
10, the impurity magnesium ion in mixed liquor, aluminium ion, iron ion can be removed after separation of solid and liquid obtains the higher calcium chloride of purity,
Solution is neutral with salt acid for adjusting pH again after separation of solid and liquid, converts calcium chloride for calcium hydroxide.
65 DEG C of flue gas exit temperature after purification, outlet sulfur dioxide concentration are 149mg/Nm3, desulfuration efficiency 85%, tail
Gas qualified discharge.Desulfurating dust-removing equipment is run 24 hours, can produce 1.1 tons of gypsum and 0.5 ton of calcium chloride dihydrate.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of method of desulfurization co-production gypsum and calcium chloride, which is characterized in that the described method comprises the following steps:
(1) epoxy propane saponified slag water logging is gone out, after leaching be separated by solid-liquid separation obtain include calcium hydroxide and calcium chloride leaching
Liquid A out；
(2) the calcium chloride mass concentration in leachate A is controlled as 25%-35%, and the pH value of leachate A is controlled as 5.3-
6.5, then using the leachate A for controlling calcium chloride concentration and pH as desulfurization absorbing liquid input in desulfuration absorbing tower with sulfur dioxide
It is mixed to obtain mixed liquid B；
(3) pH value for controlling mixed liquid B is 4.0-5.0 and aeration obtains mixture C, the gas of the aeration into mixed liquid B
In include oxygen；
(4) filtered fluid D and solid E are obtained after being separated by solid-liquid separation mixture C, will obtain gypsum after solid E drying；
(5) mixed liquor F is obtained after mixing filtered fluid D with leachate A, and mixed liquor F is allocated as part A and part B, part A control
Calcium chloride mass concentration processed is 25%-35%, pH value is that 5.3-6.5 is inhaled as the desulfurization absorbing liquid input desulfurization in step (2)
It receives in tower, prepares calcium chloride solution after the part B removal impurity of mixed liquor F, step evaporation of going forward side by side crystallizes to obtain calcium chloride.
2. the method according to claim 1, wherein the part B of mixed liquor F removes impurity in the step (5)
The method of calcium chloride solution is prepared afterwards are as follows: the pH value for adjusting the part B of mixed liquor F is 8.5-10, and it is miscellaneous to be separated by solid-liquid separation removal solid
Adjusting the pH of filtrate with hydrochloric acid after matter is that 6.5-7.5 obtains calcium chloride solution.
3. the method according to claim 1, wherein in the step (2), the chlorination in leaching liquor A is calcareous
Measuring concentration control is 30%-31%.
4. the method according to claim 1, wherein the pH value in leaching liquor A is controlled in the step (2)
It is 6.
5. the method according to claim 1, wherein in the step (3), the pH value for controlling mixed liquid B is
4.5。
6. being exposed the method according to claim 1, wherein the step (3) carries out in aeration tank or aeration tower
The gas of gas is air or oxygen.
7. the method according to claim 1, wherein in the step (2), desulfurization absorbing liquid and sulfur dioxide
Ratio is 0.5-8.0L/m3。
8. the method according to claim 1, wherein epoxy propane saponified cinder ladle includes the ingredient of following parts by weight:
Vector 20%-30%, calcium oxide 20%-65%, calcium chloride 1.57%-10.96% and impurity are burnt, institute's impurity includes that calorize is closed
Object, magnesium compound, iron compound and silicon compound.
9. the method according to claim 1, wherein in the step (2), being used to control pH's in step (3)
PH adjusting agent is acidic ph modifier, and the acidic ph modifier is hydrochloric acid.
10. according to the method described in claim 2, it is characterized in that, adjusting the part B of mixed liquor F in the step (5)
The pH adjusting agent of pH value is alkaline pH adjusting agent, and the alkaline pH adjusting agent is the leachate A of calcium hydroxide or saponification slag.
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| CN201910729421.0A CN110436505A (en) | 2019-08-07 | 2019-08-07 | A kind of method of desulfurization co-production gypsum and calcium chloride |
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| CN201910729421.0A CN110436505A (en) | 2019-08-07 | 2019-08-07 | A kind of method of desulfurization co-production gypsum and calcium chloride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115477563A (en) * | 2022-09-13 | 2022-12-16 | 葫芦岛锌业股份有限公司 | Method for preparing soil conditioner from epoxypropane saponification slag and gold dressing tailings |
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|---|---|---|---|---|
| CN203355601U (en) * | 2013-07-22 | 2013-12-25 | 山东美陵中联环境工程有限公司 | Device for treating sulfur dioxide flue gas by utilizing saponified wastewater |
| CN103482590A (en) * | 2013-07-23 | 2014-01-01 | 沈阳化工大学 | Method used for combined production of hydrazine hydrate and calcium chloride by saponification slag |
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2019
- 2019-08-07 CN CN201910729421.0A patent/CN110436505A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203355601U (en) * | 2013-07-22 | 2013-12-25 | 山东美陵中联环境工程有限公司 | Device for treating sulfur dioxide flue gas by utilizing saponified wastewater |
| CN103482590A (en) * | 2013-07-23 | 2014-01-01 | 沈阳化工大学 | Method used for combined production of hydrazine hydrate and calcium chloride by saponification slag |
Non-Patent Citations (2)
| Title |
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| 刘天齐等: "《三废处理工程技术手册 废气卷》", 31 May 1999, 化学工业出版社 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115477563A (en) * | 2022-09-13 | 2022-12-16 | 葫芦岛锌业股份有限公司 | Method for preparing soil conditioner from epoxypropane saponification slag and gold dressing tailings |
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Application publication date: 20191112 |