CN102765767B - Delay coking coke cooling water demulsifier composition and preparation method and application thereof - Google Patents
Delay coking coke cooling water demulsifier composition and preparation method and application thereof Download PDFInfo
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- CN102765767B CN102765767B CN201210245296.4A CN201210245296A CN102765767B CN 102765767 B CN102765767 B CN 102765767B CN 201210245296 A CN201210245296 A CN 201210245296A CN 102765767 B CN102765767 B CN 102765767B
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Abstract
The invention relates to a delay coking coke cooling water demulsifier composition and a preparation method and application thereof. The demulsifier composition comprises the following components in percentage by mass: 1 to 25 percent of demulsifier, 1 to 20 percent of dispersing agent, 1 to 25 percent of penetrating agent, 1 to 20 percent of corrosion inhibitor and the balance of solvent. The invention also provides the preparation method for the demulsifier composition and the application of the demulsifier composition to a delay coking device. The demulsifier composition mainly contains the demulsifier, the dispersing agent, the penetrating agent, the corrosion inhibitor and the solvent. By the demulsifier composition, the coke cooling water can be demulsified quickly, and the oil content of water can be reduced obviously; a water body is clear after demulsification; the corrosion of the water body to equipment can be reduced; and meanwhile, the demulsifier composition does not contain any inorganic ion, so that the influence on the conventional water body system is avoided.
Description
Technical field
The invention belongs to technical field of industrial sewage treatment, relate to a kind of auxiliary chemicals emulsion splitter, particularly a kind of breaker composition and preparation method thereof and application being applied to the oily(waste)water that delayed coking coke drum decoking produces.
Background technology
Delayed coking is that residual oil is converted into gas through degree of depth thermally splitting, the course of processing of matter distillate and coke in light, is that refinery improves yield of light oil and produces the Main Means of refinery coke.
The removal of coke adopts hydraulic decoking technology, coke inevitably produces the pollutents such as dust, sewage, waste gas in cooling, excision process, have a strong impact on device and environment around, particularly give greatly in water-cooled Jiao, bubble Jiao, flooding process at device, can produce large amount temperature at oil-containing, the sour water of about 100 DEG C, we are referred to as coke cooling water.Owing to originally there is emulsifying agent in crude oil, and water is made the emulsification of water body very serious by reasons such as the liftings repeatedly of pump in working cycle, causes air cooling place to block, makes follow-up sewer gas device burden simultaneously, makes the rate of loss of oil greatly increase simultaneously.Because oil quality increases the weight of day by day, the tensio-active agent used in additive in leading portion refining process is also on the increase, and makes the emulsification of water body even more serious, and the technique of crude oil much can not meet the breakdown of emulsion requirement of coke cooling water.
Patent CN2533134Y discloses a kind of coke cooling water circulation treatment devic for coking, adopts the method for the series connection of Multi-stage spiral oil eliminator and the series connection of multistage air cooler, except detergent oil and reduction water temperature.This method increase equipment pressure drop and facility investment, and floor space.There is serious blockage problem in hot water lift pump, oil eliminator etc. simultaneously, and influential system runs well.
Patent CN1754829A discloses a kind of coking sewage treatment method and device, part coke cooling water and hot coke cooling water are mixed into hot water surge tank, the part high-temperature oil gas of coke drum discharge has been cleaned while reducing sewage temperature, oil vapour pollution is decreased from source, but be increased system water amount and facility investment, cause the waste of heat.
Existing technology relates generally to and utilizes equipment to carry out break milk separation, and seldom has the report adopting and add the mode of emulsion splitter.The present invention adopts the mode of adding emulsion splitter to carry out breakdown of emulsion, and easy and simple to handle, add dosage few, can realize profit sharp separation, de-emulsification speed is fast; With the addition of inhibiter simultaneously, slow down the corrosion of equipment greatly.
Summary of the invention
The object of the invention is the deficiency overcoming prior art existence, a kind of breaker composition practical to coke cooling water is provided, source is easy to get this breaker composition composition, preparation technology is simple and add-on is few, the fast emulsion breaking of coke cooling water can be realized, significantly reduce the oleaginousness in water at 30min; Water-oil interface are clear, and after breakdown of emulsion, water body is limpid; Reduce water body to the corrosion of equipment; Simultaneously not containing mineral ion, on existing water body system without impact.
The technical scheme of employing of the present invention is as follows:
A kind of Delayed coking coke-cooling water breaker composition, the component of this breaker composition and the mass percentage content of each component are: emulsion splitter 1-25%, dispersion agent 1-20%, permeate agent 1-25%, inhibiter: 1-20%, and all the other are solvent.
Preferably, the component of this breaker composition and the mass percentage content of each component are: emulsion splitter 20-25%, dispersion agent 9-11%, permeate agent 3-6%, inhibiter: 15-18%, and all the other are solvent.
Preferably, described emulsion splitter is one or more the mixture in polyethylene polyamine propylene polyethenoxy ether (molecular weight 2000 ~ 4000), alkylphenol-formaldehyde resin polyoxyethylene poly-oxygen propylene aether (molecular weight 400 ~ 2000), alkylphenol-formaldehyde resin polyoxyethylene polyoxypropylene ether (molecular weight 1000 ~ 3000), polyethylene polyamine polyoxypropylene propylene ether (AP111, AP126, AP257).
Preferably, described dispersion agent is one or more the mixture in Sodium hexametaphosphate 99, tertiary sodium phosphate, poly aspartic acid (sodium) (molecular weight 1000 ~ 5000), hydrolytic polymaleic anhydride (molecular weight 400 ~ 800), sodium polyacrylate (molecular weight 1000 ~ 10000).
Preferably, described permeate agent is propanediol polyoxypropylene polyoxyethylene blocks polyethers (molecular weight 2000 ~ 3000), paregal O-15(C
42 ~ 48h
86 ~ 98o
16), one or more mixture of Nonyl pheno (12) ether phosphoric acid monoesters.
Preferably, described inhibiter is ethylene diamine tetra methylene phosphonic acid sodium (C
6h
12o
12n
2p
4na
8), 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (C
2h
8o
7p
2), Amino Trimethylene Phosphonic Acid (N (CH
2pO
3h
2)
3), diethylene triamine pentamethylene phosphonic (C
9h
28o
15n
3p
5), one or more mixture in polyamino polyether base methylenephosphonic acid (molecular weight about 600, molecular formula is as follows).
Preferably, described solvent is deionized water.
The preparation method that present invention also offers above-mentioned breaker composition is: by above-mentioned weight percent, emulsion splitter, dispersion agent, permeate agent, inhibiter, solvent are added to vessel in heating (or not heating), after being uniformly mixed, be cooled to room temperature, obtain breaker composition product.
Present invention also offers the application of above-mentioned breaker composition in delayed coking unit.
Preferably, the delayed coking unit that it is raw material that breaker composition of the present invention is applicable to paraffinic base, intermediate base, naphthenic residual oil.
Present invention also offers the using method of above-mentioned breaker composition, during use, after emulsion splitter is joined water cooling plant before gun barrel, add-on is the 100-200ppm of coke cooling water.
The beneficial effect that the present invention has:
Breaker composition of the present invention is mainly containing emulsion splitter, dispersion agent, permeate agent, inhibiter and solvent.Breaker composition of the present invention can realize the fast emulsion breaking of coke cooling water, significantly reduces the oleaginousness in water; After breakdown of emulsion, water body is limpid; Reduce water body to the corrosion of equipment; Simultaneously not containing mineral ion, on existing water body system without impact.
Breaker composition good water solubility of the present invention, can dissolve each other fast with sour water; Filling is convenient, does not affect the normal production of device, does not affect quality product.
Embodiment
By the following examples technical scheme of the present invention is described further, but does not limit protection scope of the present invention.
Embodiment 1
A kind of preparation method of breaker composition, comprise the steps: 160g polyethylene polyamine propylene polyethenoxy ether (16%), 200g Sodium hexametaphosphate 99 (20%), 140g propanediol polyoxypropylene polyoxyethylene blocks polyethers (14%), 120g ethylene diamine tetra methylene phosphonic acid sodium (12%), 380g deionized water (38%), is added to after being uniformly mixed in container, be cooled to room temperature, filter and obtain breaker composition A product.
Embodiment 2
A kind of preparation method of breaker composition, comprise the steps: 250g alkylphenol-formaldehyde resin polyoxyethylene poly-oxygen propylene aether (25%), 200g tertiary sodium phosphate (20%), 250g propanediol polyoxypropylene polyoxyethylene blocks polyethers (25%), 200g ethylene diamine tetra methylene phosphonic acid sodium (20%), 100g deionized water (10%), is added to after being uniformly mixed in container, be cooled to room temperature, filter and obtain breaker composition B product.
Embodiment 3
A kind of preparation method of breaker composition, comprise the steps: 120g alkylphenol-formaldehyde resin polyoxyethylene poly-oxygen propylene aether (12%), 200g poly aspartic acid (sodium) (20%), 120g paregal O-15(12%), 110g 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (11%), 450g deionized water (45%), be added to vessel in heating, after being uniformly mixed, be cooled to room temperature, filter and obtain breaker composition C product.
Embodiment 4
A kind of preparation method of breaker composition, comprise the steps: 180g alkylphenol-formaldehyde resin polyoxyethylene polyoxypropylene ether (18%), 180g tertiary sodium phosphate (18%), 130g propanediol polyoxypropylene polyoxyethylene blocks polyethers (13%), 100g 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (10%), 410g deionized water (41%), is added to after being uniformly mixed in container, be cooled to room temperature, filter and obtain breaker composition D product.
Embodiment 5
A kind of preparation method of breaker composition, comprise the steps: 140g alkylphenol-formaldehyde resin polyoxyethylene polyoxypropylene ether (14%), 160g poly aspartic acid (sodium) (16%), 110g Nonyl pheno (12) ether phosphoric acid monoesters (11%), 200g diethylene triamine pentamethylene phosphonic (20%), 390g deionized water (39%), be added to vessel in heating, after being uniformly mixed, be cooled to room temperature, filter and obtain breaker composition E product.
Embodiment 6
A kind of preparation method of breaker composition, comprise the steps: 150g polyethylene polyamine polyoxypropylene propylene ether (15%), 200g hydrolytic polymaleic anhydride (20%), 110g paregal O-15(11%), 120g 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (12%), 420g deionized water (42%), be added to vessel in heating, after being uniformly mixed, be cooled to room temperature, filter and obtain breaker composition F product.
Embodiment 7
A kind of preparation method of breaker composition, comprise the steps: 10g polyethylene polyamine propylene polyethenoxy ether (1%), 10g hydrolytic polymaleic anhydride (1%), 10g Nonyl pheno (12) ether phosphoric acid monoesters (1%), 10g diethylene triamine pentamethylene phosphonic (1%), 960g deionized water (96%), be added to vessel in heating, after being uniformly mixed, be cooled to room temperature, filter and obtain breaker composition G product.
Embodiment 8
A kind of preparation method of breaker composition, comprise the steps: 125g polyethylene polyamine polyoxypropylene propylene ether (12.5%), 100g Sodium hexametaphosphate 99 (10%), 125g propanediol polyoxypropylene polyoxyethylene blocks polyethers (12.5%), 100g 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (15%), 500g deionized water (50%), be added to vessel in heating, after being uniformly mixed, be cooled to room temperature, filter and obtain breaker composition H product.
Embodiment 9
A kind of preparation method of breaker composition, comprise the steps: 250g alkylphenol-formaldehyde resin polyoxyethylene polyoxypropylene ether (25%), 100g poly aspartic acid (sodium) (10%), 50g propanediol polyoxypropylene polyoxyethylene blocks polyethers (5%), 150g diethylene triamine pentamethylene phosphonic (15%), 450g deionized water (45%), is added to after being uniformly mixed in container, be cooled to room temperature, filter and obtain breaker composition I product.
Embodiment of the present invention 1-9 is the lab scale of breaker composition for Delayed coking coke-cooling water effect, tests respectively with regard to the different dosage of 50ppm, 100ppm, 150ppm, 200ppm to each product of Delayed coking coke-cooling water breaker composition.
By coke-cooling waste water (fetching water during little feedwater), carry out quantitative separating, every 100g water sample one glass, quantitatively being added drop-wise to by identical dosage by the breaker composition of embodiment 1-9 respectively fills in the beaker of coke cooling water, stir 5min, rotating speed 350r/min, after timing 30min, carries out the measurement of water body oleaginousness, COD.Pilot run is in Table 1-4.
Table 1 dosage is 50ppm test-results
Table 2 dosage is 100ppm test-results
Table 2 dosage is 150ppm test-results
Table 3 dosage is 200ppm test-results
The blank control group for not adding breaker composition, can find out along with the oleaginousness of emulsion splitter dosage, the removal trend of COD obviously increase from pilot run, the effect considering I product is better compared with other products.
The concrete detection method of oleaginousness, COD:
COD detects needs instrument and medicine:
The Erlenmeyer flask of instrumented medication: 500ml, Electric stove, prolong, Mercury bisulfate, the vitriol oil, sulfuric acid-silver sulfate solution, phenanthroline ion indicator, potassium bichromate standardized solution, ferrous ammonium sulphate standardized solution, graduated cylinder, distilled water.
COD detection method:
0.5g Mercury bisulfate is added in the Erlenmeyer flask of 500ml, add the liquid to be measured after dilution (5ml liquid to be measured adds the distilled water diluting of 20ml) 25ml, add vitriol oil 10ml, shake up, measure potassium bichromate standardized solution 10ml to add in the liquid to be measured prepared, then add the sulfuric acid-silver sulfate solution of 40ml, shake up, after starting to be heated to boiling, during add-back flowmeter 5 minutes.
With the distilled water flushing prolong of 100ml after its cooling, overall solution volume is made to be no less than 140ml.
Add 3 phenanthroline ion indicator after solution cools completely, with the titration of ferrous ammonium sulphate standardized solution, solution is titration end point by yellow through blue-greenish colour to sorrel, and record consumes mark liquid and amasss.
Replace all the other steps of liquid to be measured after dilution identical with step during test liquid to be measured with 25ml distilled water time blank.
Calculate: COD=(V
0-V
1) × C × 8 × 1000/V
The volumetric molar concentration (mol/L) of C------ferrous ammonium sulphate standardized solution in formula
V
0the volume (ml) of ferrous ammonium sulphate is consumed when-------titration is blank
V
1the volume (ml) of ferrous ammonium sulphate is consumed during-----titration liquid to be measured
The volume (ml) of V-------liquid to be measured
8-------oxygen (1/20) molar mass (g/mol)
Oleaginousness detects: laboratory apparatus medicine:
The sherwood oil of 60 ~ 90 DEG C of boiling points, analytical pure NaCl, water sample to be measured, electronic balance (being accurate to 0.01g), 250ml separating funnel one, small beaker three, two, 50ml measuring cup, constant temperature roaster.
Oleaginousness detection method
1. take 2 ~ 3gNaCl with electronic balance and pour separating funnel into, then get a beaker, weighed amount ml, and perform mark.
2. measure 20ml water sample to be measured with measuring cup, pour separating funnel into.
3. get 10 ~ 12ml sherwood oil with another measuring cup and pour separating funnel into.
4. funnel upper end glass plug withstands by right hand forefinger minor details, then holds funnel with thumb and forefinger and middle finger, and left-handed forefinger and middle finger are curled up and be held on the handle of piston, up and down jolting separating funnel gently, makes fully to contact between two-phase, to improve extraction efficiency.After every jolting several times, funnel afterbody will be inclined upwardly (towards unmanned place) open piston venting, to remove the pressure in funnel.After only having very little pressure when repetition like this is extremely exitted, more violent jolting 2 ~ 3min, leave standstill, after two-phase is separated completely, open Bo Sai above, then piston is slowly outwarded winding, lower floor's liquid is released from piston, sometimes alternately may occur that some flosss also should be put simultaneously two.Then supernatant liquid being weighed up the small beaker of weight from suitable for reading the pouring into of separating funnel, putting into oven cooking cycle to no longer including liquid substance.
5. take the complete small beaker of baking and solid matter gross weight m2.
Calculate: oleaginousness (mg/l)=(m2-m1)/v × 106
In formula: ml and m2 unit is g, v=20ml
The above is only preferred embodiment of the present invention, not does any pro forma restriction to technical scheme of the present invention.Every above embodiment is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all still belong in the scope of technical scheme of the present invention.
Claims (5)
1. a Delayed coking coke-cooling water breaker composition, is characterized in that: the component of this breaker composition and the mass percentage content of each component are: emulsion splitter 1-25%, dispersion agent 1-20%, permeate agent 1-25%, inhibiter: 1-20%, and all the other are solvent;
Described emulsion splitter is molecular weight is 2000 ~ 4000 polyethylene polyamine propylene polyethenoxy ethers, molecular weight is 400 ~ 2000 alkylphenol-formaldehyde resin polyoxyethylene poly-oxygen propylene aethers, molecular weight is one or more mixture in 1000 ~ 3000 alkylphenol-formaldehyde resin polyoxyethylene polyoxypropylene ethers, polyethylene polyamine polyoxypropylene propylene ether AP111, AP126, AP257;
Described dispersion agent is Sodium hexametaphosphate 99, tertiary sodium phosphate, molecular weight are 1000 ~ 5000 poly (sodium aspartate)s, molecular weight is 400 ~ 800 hydrolytic polymaleic anhydride, molecular weight is one or more mixture in 1000 ~ 10000 sodium polyacrylates;
Described permeate agent is molecular weight is 2000 ~ 3000 propanediol polyoxypropylene polyoxyethylene blocks polyethers, paregal O-15 (C
42 ~ 48h
86 ~ 98o
16), one or more mixture of Nonyl pheno (12) ether phosphoric acid monoesters;
Described inhibiter is one or more the mixture in ethylene diamine tetra methylene phosphonic acid sodium, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, Amino Trimethylene Phosphonic Acid, diethylene triamine pentamethylene phosphonic, polyamino polyether base methylenephosphonic acid;
Described solvent is deionized water.
2. a kind of Delayed coking coke-cooling water breaker composition according to claim 1, it is characterized in that: the component of this breaker composition and the mass percentage content of each component are: emulsion splitter 20-25%, dispersion agent 9-11%, permeate agent 3-6%, inhibiter: 15-18%, all the other are solvent.
3. the preparation method of breaker composition described in claim 1 or 2, it is characterized in that: by above-mentioned weight percent, emulsion splitter, dispersion agent, permeate agent, inhibiter, solvent are added to vessel in heating or do not heat, after being uniformly mixed, be cooled to room temperature, obtain breaker composition product.
4. the application of breaker composition described in claim 1 or 2 in delayed coking unit.
5. the using method of breaker composition described in claim 1 or 2, is characterized in that: during use, and after breaker composition is joined water cooling plant before gun barrel, add-on is the 100-200ppm of coke cooling water.
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| CN103951009A (en) * | 2014-02-17 | 2014-07-30 | 宜兴汉光高新石化有限公司 | Coking demulsifier and preparation method thereof |
| CN104176788B (en) * | 2014-09-09 | 2015-11-04 | 中国石油化工股份有限公司 | A kind of degreaser for oil field binary combination flooding produced sewerage and preparation method thereof |
| CN105540738B (en) * | 2015-12-17 | 2017-12-08 | 广州小众环保科技有限公司 | A kind of efficient demulsifier and its preparation method and application |
| CN109133405B (en) * | 2017-06-19 | 2021-10-08 | 中国石油化工股份有限公司 | Method for purifying sulfur-containing sewage of delayed coking |
| CN112480945A (en) * | 2020-10-30 | 2021-03-12 | 长江大学 | Rice hull charcoal, demulsifier, preparation method and application thereof |
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