CN108854165A - Oily separation method in a kind of deammoniation tower ammonia lime set - Google Patents
Oily separation method in a kind of deammoniation tower ammonia lime set Download PDFInfo
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- CN108854165A CN108854165A CN201711462269.1A CN201711462269A CN108854165A CN 108854165 A CN108854165 A CN 108854165A CN 201711462269 A CN201711462269 A CN 201711462269A CN 108854165 A CN108854165 A CN 108854165A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0205—Separation of non-miscible liquids by gas bubbles or moving solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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Abstract
The present invention relates to separation methods oily in a kind of deammoniation tower ammonia lime set, include the following steps, 1）Ammonia lime set after deammoniation tower is sent into neutralizing tower, acidic materials are added in the ammonia lime set into neutralizing tower and react to form ammonium salt and reach oily aqueous phase separation；2）Oil is mutually sent to light oil tank after dividing oil tank, in aqueous-phase reflux to extracting tower or deammoniation tower.Acidic materials are added into ammonia lime set to be neutralized, form ammonium salt, increase aqueous phase densities, there is salting out simultaneously, air bearing effect can be generated by being passed through sour gas also, make it is oily mutually and the layering of water phase, convenient for oil is separated, solve grease in ammonia lime set can not separate, waste can, organic matter is enriched in ammonia and can break the balance of system components within a certain period of time and impact the operation problem of phenol tower and biochemical treatment system.
Description
Technical field
The present invention relates at coal chemical industry, lurgi gasifier, crushed coal pressurized-gasification furnace, BGL furnace and coking and semi-coke industry waste water
A kind of science and engineering skill, and in particular to oily separation method in deammoniation tower ammonia lime set.
Background technique
Coal chemical industry, coking and gasification wastewater, coke-stove gas waste water and semi-coke coal gas waste in semi-coke industry refer to that coal exists
To the very high waste water of pollutant concentration generated after the separation of gas washing, condensation and gas liquor in gasification or retort process, contain
A large amount of phenol, ammonia, cyanide and oil etc..It, will also be using physico-chemical process to recoverable in waste water before entering biochemical treatment
Substance, such as phenol, ammonia are recycled.Its technique is generally gas liquor separation-depickling-deamination-phenol extraction-biochemical treatment or coal
Gas-water separation-deamination-depickling-phenol extraction-biochemical treatment.
By taking gas liquor separation-depickling-deamination-phenol extraction-biochemical processing process as an example, waste water after gas liquor separates, into
Enter the sour gas such as extracting tower carbon dioxide removal and hydrogen sulfide, removes ammonia subsequently into deammoniation tower, it is de- to enter back into phenol extraction tower
Phenol eventually enters into biochemical treatment system.In deammoniation tower workshop section, there are level-one, second level, three-level condenser and liquid separation tank, it is final to obtain
To 98% or so ammonia.Ammonia content is up to 7% in lime set after liquid separation tank, therefore referred to as ammonia lime set.Enter after ammonia lime set is cooling and divides
Oil tank carries out water-oil separating, wherein isolated oil, which is sent to light oil tank most Zhongdao tank field, water phase, then flows back into deammoniation tower.
But in actual production, 125-140 DEG C of deamination column overhead temperatures slip out component in addition to ammonia and steam, and there are also big
The organic component of amount, and be mostly hydrophilic organics hydrophilicity, it has been investigated that containing nitrile, pyridines, aromatic hydrocarbons, alcohols, phenols
Deng.It is almost not stratified in emulsification oil condition in ammonia lime set weak aqua ammonia medium because these organic concentrations are higher.Therefore its ammonia is solidifying
Liquid divides oil tank almost not work, the oil aqueous 90% or more being sent in light oil tank, can not be sent to tank field take-away, typically heavy
Newly send coal gas water separation device circular treatment again back to.And the ammonia lime set water phase flowed back into after point oil of deammoniation tower is in milkiness shape,
Therefore these lightweight organic component light oil actually distilled out from deammoniation tower recycle in system repeatedly.Not only cause system in vain
Energy consumption, and cause content of organics in the ammonia of recycling high, while the oil of these return systems repeatedly runs up to certain journey
Degree, will break the vapor liquid equilibrium of system, these light oils is caused to enter phenol extraction tower, phenol tower extraction efficiency is caused to decline to a great extent,
Phenol and COD in water outlet（COD）Content substantially exceeds design value, the operation of serious impact downstream biochemical treatment system.
Summary of the invention
The present invention can not separate for grease in ammonia lime set, waste energy, organic matter is enriched with and in certain time in ammonia
The interior balance that can break system components and the operation problem for impacting phenol tower and biochemical treatment system, provide a kind of deammoniation tower ammonia lime set
The separation method of middle oil.
Oily separation method adopts the following technical scheme that in a kind of deammoniation tower ammonia lime set of the invention：A kind of deammoniation tower ammonia is solidifying
Oily separation method, includes the following steps in liquid,
1）Ammonia lime set in deammoniation tower is sent into neutralizing tower, acidic materials are added in the ammonia lime set into neutralizing tower and react shape
Reach oily aqueous phase separation at ammonium salt；
2）Oil is mutually sent to light oil tank after being divided oil tank water-oil separating, in aqueous-phase reflux to extracting tower or deammoniation tower.
The ammonia lime set be level-one ammonia lime set, secondary amine lime set, tertiary amine lime set, divide it is any in the ammonia lime set in oil tank
It is one or more of.
The acidic materials are liquid acid or sour gas.
The liquid acid is hydrochloric acid, any one or two kinds in sulfuric acid.
The sour gas is CO2、H2Any one in S or two kinds.
The sour gas is from purification device or extracting tower.
The sour gas is passed through from the bottom of neutralizing tower, and excessive sour gas enters scrubbing tower by neutralizing tower top,
It is sent after the next phenol water washing of deamination tower bottom to sulfur recovery unit processing, the ammonia lime set pH value after sour gas is saturated is weak
Alkalinity is simultaneously from tower bottom discharge is neutralized, and after being divided oil tank water-oil separating, upper oil phase is sent to light oil tank, water phase then with scrubbing tower bottom
Waste water out flows back into extracting tower together.
The liquid acid is added from the top of neutralizing tower, and the ammonia lime set pH value after acidification is 5-9 and from neutralizing tower bottom
Portion's discharge, after dividing oil tank, upper oil phase is sent to light oil tank, aqueous-phase reflux to deammoniation tower.
The liquid acid uses concentration for 1:1 sulfuric acid or concentration are 1:1 hydrochloric acid.
The sour gas is the CO from purification device2, the ammonia lime set pH value after sour gas is saturated is 8.0-
9.5；Or sour gas is the mixed gas in extracting tower, CO in mixed gas2Mass fraction be 96.2%, H2S
Mass fraction be 1.1%, sour gas saturation after ammonia lime set pH value be 8.0-9.5.
The beneficial effects of the invention are as follows：Acidic materials are added into ammonia lime set to be neutralized, forms ammonium salt, increases water phase
Density, while there is salting out, so that the layering of oily phase and water phase is solved grease in ammonia lime set convenient for separating oil
It can not separate, waste energy, organic matter is enriched in ammonia and can break the balance of system components within a certain period of time and impact phenol
The operation problem of tower and biochemical treatment system.
Further, acidic materials use sour gas, and the process that is passed through of sour gas has air bearing effect, make newborn in ammonia lime set
Carburetion floats with oily unstability is partly dissolved, and realizes the separation of oil and water.
Detailed description of the invention
Fig. 1 be acidic materials be liquid acid when process flow chart；
Fig. 2 be acidic materials be sour gas when process flow chart.
Specific embodiment
The invention is further explained in the following combination with the attached drawings of the specification：
Embodiment 1：
As shown in Figure 1, include the following steps, neutralizing tower is sent by the ammonia lime set in deammoniation tower, from the top of neutralizing tower to neutralization
It is 1 that concentration is added dropwise in ammonia lime set in tower:1 sulfuric acid, stirring, until the pH value of ammonia lime set stands 30 minutes, upper layer in 5-9
Light oil is sent to light oil tank, and lower layer's water phase flows back into deammoniation tower, then subsequent by phenol extraction tower progress phenol removal.In ammonia lime set
Add liquid acid（1:1 sulfuric acid）It neutralizes, forms ammonium salt, increase aqueous phase densities, simultaneous salting-out effect makes on light oil
It is floating, it preferably solves the separation problem of grease in ammonia lime set, ensure that the stable operation of system, obtained light oil produces bright
Aobvious economic benefit, the stable operation for the recycling of subsequent phenol and biochemical treatment provide guarantee.
It is 1 that concentration is added dropwise into ammonia lime set for table 1:Data comparison before and after 1 sulfuric acid treatment
| Waste water | The amount of oil is precipitated | COD | Total phenol | PH value | Appearance |
| Stoste | 0 g/L | 10.36g/L | 22.66 g/L | 10.5 | It is muddy |
| After acid is added dropwise | 11g/L | 6.34 g/L | 16.1 g/L | 5.5 | There is milky |
Embodiment 2：
As shown in Figure 1, including the following steps, by the ammonia lime set feeding neutralizing tower in deammoniation tower, in the ammonia lime set into neutralizing tower
It is 1 that concentration, which is added dropwise,:1 hydrochloric acid, stirring, until the pH value of ammonia lime set stands 30 minutes in 5-9, upper layer light oil is sent to light oil tank,
Lower layer's water phase flows back into deammoniation tower, then subsequent by phenol extraction tower progress phenol removal.Liquid acid is added in ammonia lime set（1:1
Hydrochloric acid）It neutralizes, forms ammonium salt, increase aqueous phase densities, simultaneous salting-out effect makes light oil float, and preferably solves
The separation problem of grease in ammonia lime set, ensure that the stable operation of system, and obtained light oil produces apparent economic benefit, be
The stable operation of subsequent phenol recycling and biochemical treatment provides guarantee.
It is 1 that concentration is added dropwise into ammonia lime set for table 2:Data comparison before and after 1 HCl treatment
| Waste water | The amount of oil is precipitated | COD | Total phenol | PH value | Appearance |
| Stoste | 0 g/L | 8.66g/L | 18.7 g/L | 10.0 | It is muddy |
| After acid is added dropwise | 12.3 g/L | 5.60 g/L | 13.3 g/L | 8.2 | Slight milky |
Embodiment 3：
As shown in Fig. 2, including the following steps, neutralizing tower is sent by the ammonia lime set in deammoniation tower, the titanium dioxide come from purification device
Carbon gas enters in tower from the bottom of neutralizing tower, and carbon dioxide gas is absorbed into waste water by ammonia lime set, excessive titanium dioxide
Carbon gas enters in scrubbing tower from top of tower is neutralized, and is further sent sulfur recovery to fill after the dilute phenol water washing come in phenol extraction tower
Set processing.Ammonia lime set pH value after sour gas saturation is 9.1, and from neutralization tower bottom discharge, the upper oil phase after dividing oil tank
It is sent to light oil tank, the waste water that water phase then comes out with wash tower bottoms flows back into extracting tower together.Dioxy is passed through in ammonia lime set
Change carbon gas to be neutralized, forms ammonium salt, increase aqueous phase densities, simultaneous salting-out effect makes light oil float, and dioxy
The process that is passed through for changing carbon gas has air bearing effect, preferably solves the separation problem of grease in ammonia lime set, ensure that system
Stable operation, obtained light oil produce apparent economic benefit, and the stable operation for the recycling of subsequent phenol and biochemical treatment provides
It ensures.
Table 3 enters data comparison before and after the carbon dioxide treatment that purification device comes into ammonia lime set
| Waste water | The amount of oil is precipitated | COD | Total phenol | PH value | Appearance |
| Stoste | 0 g/L | 9.98 g/L | 19.4 g/L | 10.2 | It is muddy |
| After being passed through CO2 | 11.0 g/L | 6.53 g/L | 12.6 g/L | 9.1 | Limpid micro- Huang |
Embodiment 4：
As shown in Fig. 2, including the following steps, neutralizing tower is sent by the ammonia lime set in deammoniation tower, the mixing come from depickling tower apparatus
Gas, main component is CO in mixed gas2And H2S, wherein CO2Mass fraction be 96.2%, H2The mass fraction of S is
1.1%, remaining ingredient is steam, is entered in tower from the bottom of neutralizing tower, sour gas is absorbed into waste water by ammonia lime set, mistake
The sour gas of amount enters in scrubbing tower from top of tower is neutralized, and is further sent sulphur to return after the phenol water washing come in phenol extraction tower
Receiving apparatus processing.Ammonia lime set pH value after sour gas saturation is 8.8, and from tower bottom discharge is neutralized, upper layer is oily after dividing oil tank
It is mutually sent to light oil tank, the waste water that water phase then comes out with scrubbing tower bottom flows back into extracting tower together.Dioxy is passed through in ammonia lime set
The mixed gas for changing carbon and hydrogen sulfide is neutralized, and is formed ammonium salt, is increased aqueous phase densities, simultaneous salting-out effect makes gently
Oil floats, and the process that is passed through of mixed gas has air bearing effect, preferably solves the separation problem of grease in ammonia lime set, guarantees
The stable operation of system, obtained light oil produce apparent economic benefit, for the stabilization of subsequent phenol recycling and biochemical treatment
Operation provides guarantee.Further, original device is utilized（Extracting tower）The sour gas of generation is neutralized, and is made full use of
Existing apparatus and raw material, do not generate waste additionally, not only save equipment investment and cost of material, Er Qiehuan after processing
It protects.
Table 4 is passed through data comparison before and after the mixing Sour gas disposal that depickling tower apparatus comes into ammonia lime set
| Waste water | The amount of oil is precipitated | COD | Total phenol | PH value | Appearance |
| Stoste | 0 g/L | 9.98 g/L | 19.4 g/L | 10.5 | It is muddy |
| After being passed through mixing sour gas | 9.3 g/L | 6.62 g/L | 11.8 g/L | 8.8 | Limpid micro- Huang |
In conclusion added in ammonia lime set in acidic materials and, form ammonium salt, increase aqueous phase densities, simultaneous salt
Analysis effect makes light oil float, and the process that is passed through of sour gas has air bearing effect, preferably solves point of grease in ammonia lime set
From problem, the stable operation of system ensure that, obtained light oil produces apparent economic benefit, for the recycling of subsequent phenol and biochemistry
The stable operation of processing provides guarantee.
The present invention solves the problems, such as ammonia lime set water-oil separating, has the following advantages that：
1. effectively having recycled the oils in ammonia lime set, 10kg or so oily substance, COD removal rate can be precipitated in every side's ammonia lime set
34.52%, total phenol removal rate 28.86%.Water content in oil content≤3% after separation can directly be taken out in tank sending area.
2. reducing content of organics in ammonia.
3. the light oil for avoiding enrichment enters phenol recyclable device, the stable operation and water outlet of phenol recyclable device ensure that
Qualification rate, to stabilize the operation of biochemical treatment system.
4. effectively preventing these light oils to recycle in the device repeatedly, energy consumption can be greatly lowered.
5. utilizing original device（Extracting tower）The sour gas of generation is neutralized, and take full advantage of existing apparatus and
Raw material does not generate waste additionally after processing, not only save equipment investment and cost of material, and environmental protection.
By the wastewater flow rate that a set of 13.3 hundred million side gas plant generates, the ammonia lime set amount generated through deammoniation tower is design value 25
Cubic meter/hour, it may separate out 6 tons of light oils daily, by operating in annual 300 days and 2000 yuan per ton calculating, annual generation is direct
Economic benefit 3,600,000.
Process above process in the specific implementation process, can add instrument, such as electromagnetic flowmeter, pH meter are in fact as needed
When adjust water in the dosage of liquid acid or sour gas, realize the automation control of technique.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (10)
1. oily separation method in a kind of deammoniation tower ammonia lime set, which is characterized in that include the following steps,
1）Deammoniation tower ammonia lime set is sent into neutralizing tower, acidic materials are added in the ammonia lime set into neutralizing tower and react to form ammonium
Salt reaches oily aqueous phase separation；
2）Oil is mutually sent to light oil tank after being divided oil tank water-oil separating, in aqueous-phase reflux to extracting tower or deammoniation tower.
2. separation method according to claim 1, which is characterized in that the ammonia lime set is level-one ammonia lime set, secondary amine is solidifying
Liquid, tertiary amine lime set divide any one or a few in the ammonia lime set in oil tank.
3. separation method according to claim 1, which is characterized in that the acidic materials are liquid acid or sour gas.
4. separation method according to claim 3, it is characterised in that：The liquid acid is hydrochloric acid, any one in sulfuric acid
Kind or two kinds.
5. separation method according to claim 3, it is characterised in that：The sour gas is CO2、H2Any one in S
Or two kinds.
6. separation method according to claim 5, it is characterised in that：The sour gas is from purification device or depickling
Tower.
7. separation method according to claim 3, it is characterised in that：The sour gas is passed through from the bottom of neutralizing tower,
Excessive sour gas is returned by entering scrubbing tower at the top of neutralizing tower by sending after the next dilute phenol water washing of phenol extraction tower bottom to sulphur
Receiving apparatus processing, the ammonia lime set pH value after sour gas is saturated is alkalescent and is discharged from tower bottom is neutralized, and is divided oil tank grease
After separation, upper oil phase is sent to light oil tank, and the waste water that water phase then comes out with scrubbing tower bottom flows back into extracting tower together.
8. separation method according to claim 3, it is characterised in that：The liquid acid is added from the top of neutralizing tower, acid
Changing treated ammonia lime set pH value is 5-9 and from tower bottom discharge is neutralized, and after dividing oil tank, upper oil phase is sent to light oil tank, water
Mutually it is back to deammoniation tower.
9. separation method according to claim 4, it is characterised in that：The liquid acid uses concentration for 1:1 sulfuric acid is dense
Degree is 1:1 hydrochloric acid.
10. separation method according to claim 6, it is characterised in that：The sour gas is from purification device
CO2, the ammonia lime set pH value after sour gas is saturated is 8.0-9.5；Or sour gas is the gaseous mixture in extracting tower
Body, CO in mixed gas2Mass fraction be 96.2%, H2The mass fraction of S is 1.1%, the ammonia lime set after sour gas saturation
PH value is 8.0-9.5.
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Cited By (2)
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| CN112723383A (en) * | 2020-12-01 | 2021-04-30 | 安徽金禾实业股份有限公司 | Method for recovering sewage gas of synthetic high-pressure system |
| CN115196805A (en) * | 2022-07-21 | 2022-10-18 | 中国科学院山西煤炭化学研究所 | Treatment method for deoiling, dedusting, deacidifying and deaminating semi-coke wastewater |
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Application publication date: 20181123 |