CN102765767A - 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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- CN102765767A CN102765767A CN2012102452964A CN201210245296A CN102765767A CN 102765767 A CN102765767 A CN 102765767A CN 2012102452964 A CN2012102452964 A CN 2012102452964A CN 201210245296 A CN201210245296 A CN 201210245296A CN 102765767 A CN102765767 A CN 102765767A
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- emulsion splitter
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- cooling water
- coke cooling
- delayed coking
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- 239000000203 mixture Substances 0.000 title claims abstract description 34
- 239000000571 coke Substances 0.000 title claims abstract description 30
- 239000000498 cooling water Substances 0.000 title claims abstract description 24
- 238000004939 coking Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000000839 emulsion Substances 0.000 claims description 72
- -1 polyethylene Polymers 0.000 claims description 34
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 19
- 230000003111 delayed effect Effects 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 15
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- 239000012466 permeate Substances 0.000 claims description 9
- 229920000570 polyether Polymers 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000004698 Polyethylene Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229920000768 polyamine Polymers 0.000 claims description 8
- 229920000573 polyethylene Polymers 0.000 claims description 8
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 8
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229920001451 polypropylene glycol Polymers 0.000 claims description 7
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical group CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 7
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 5
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 5
- VHSHLMUCYSAUQU-UHFFFAOYSA-N 2-hydroxypropyl methacrylate Chemical compound CC(O)COC(=O)C(C)=C VHSHLMUCYSAUQU-UHFFFAOYSA-N 0.000 claims description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 4
- 229940120146 EDTMP Drugs 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 claims description 4
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 239000002270 dispersing agent Substances 0.000 abstract 2
- 239000003112 inhibitor Substances 0.000 abstract 2
- 230000000149 penetrating effect Effects 0.000 abstract 2
- 229910001410 inorganic ion Inorganic materials 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 15
- 239000007788 liquid Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 239000010865 sewage Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 3
- 210000005224 forefinger Anatomy 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- DOBUSJIVSSJEDA-UHFFFAOYSA-L 1,3-dioxa-2$l^{6}-thia-4-mercuracyclobutane 2,2-dioxide Chemical compound [Hg+2].[O-]S([O-])(=O)=O DOBUSJIVSSJEDA-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- YUVLVONHNMXKBW-UHFFFAOYSA-L [Ag+2].OS(O)(=O)=O.[O-]S([O-])(=O)=O Chemical compound [Ag+2].OS(O)(=O)=O.[O-]S([O-])(=O)=O YUVLVONHNMXKBW-UHFFFAOYSA-L 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 238000005235 decoking Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 210000003811 finger Anatomy 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910000372 mercury(II) sulfate Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000013022 venting Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 235000001018 Hibiscus sabdariffa Nutrition 0.000 description 1
- 235000005291 Rumex acetosa Nutrition 0.000 description 1
- 240000007001 Rumex acetosella Species 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000013527 degreasing agent Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 235000003513 sheep sorrel Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 210000003813 thumb Anatomy 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Landscapes
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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 the industrial sewage treatment technology field, relate to a kind of auxiliary chemicals emulsion splitter, particularly a kind of emulsion splitter composition and method of making the same and application that is applied to the oily(waste)water of delayed coking coke drum decoking generation.
Background technology
Delayed coking is that residual oil is converted into gas through degree of depth thermally splitting, and the course of processing of light middle matter distillate and coke is that refinery improves yield of light oil and the main means of producing refinery coke.
The hydraulic decoking technology is adopted in the removal of coke; Coke can produce pollutents such as dust, sewage, waste gas inevitably in cooling, excision process; Have a strong impact on device and environment on every side; Particularly installing big giving in water-cooled Jiao, bubble Jiao, the flooding process, can produce oil-containing, the sour water of big amount temperature about 100 ℃, we are referred to as coke cooling water.Owing to had emulsifying agent originally in the crude oil, reach water and in working cycle, made that by the reasons such as lifting repeatedly of pump the emulsification of water body is very serious, cause the air cooling place to stop up, make simultaneously the rate of loss of oil to be increased follow-up sewage gas device burden greatly.Because oil quality increases the weight of day by day, the tensio-active agent of using in the additive in the leading portion refining process also is on the increase, and makes that the emulsification of water body is even more serious, and the technology of crude oil much can not satisfy the breakdown of emulsion requirement of coke cooling water.
Patent CN2533134Y discloses a kind of coke-cooling waste water cyclic processing device, adopts multistage degreaser cyclone series connection and the placed in-line method of multistage air cooler, removes detergent oil and reduces water temperature.This method has increased equipment pressure drop and facility investment, and floor space.There are serious blockage problem in hot water lift pump, oil eliminator etc. simultaneously, and the system that influences 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 the hot water surge tank; When reducing sewage temperature, cleaned the part high-temperature oil gas of coke drum discharging; Reduce oil vapour pollution from the source, but increased system water amount and facility investment, caused the waste of heat.
Existing technology relates generally to utilizes equipment to carry out the breakdown of emulsion separation, and the report that adopts the mode that adds emulsion splitter is seldom arranged.The present invention adopts the mode of adding emulsion splitter to carry out breakdown of emulsion, and easy and simple to handle, it is few to add dosage, can realize the profit sharp separation, and de-emulsification speed is fast; Add inhibiter simultaneously, slowed down corrosion on Equipment greatly.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists; Provide a kind of to the practical emulsion splitter compsn of coke cooling water; This emulsion splitter compsn composition source is easy to get, preparation technology is simple and add-on is few; Can realize the fast emulsion breaking of coke cooling water, significantly reduce the oleaginousness in the water at 30min; Water-oil interface are clear, and water body is limpid behind the breakdown of emulsion; Reduce water body to corrosion on Equipment; Do not contain simultaneously mineral ion, existing water body system is not had influence.
The technical scheme of employing of the present invention is following:
A kind of delayed coking coke cooling water emulsion splitter compsn, the component of this emulsion splitter compsn and the mass percentage content of each component are: emulsion splitter 1-25%, dispersion agent 1-20%, permeate agent 1-25%, inhibiter: 1-20%, all the other are solvent.
Preferably, the component of this emulsion splitter compsn and the mass percentage content of each component are: emulsion splitter 20-25%, and dispersion agent 9-11%, permeate agent 3-6%, inhibiter: 15-18%, all the other are solvent.
Preferably, said 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), the polyethylene polyamine polyoxypropylene propylene ether (AP111, AP126, AP257).
Preferably, said dispersion agent is one or more the mixture in Sodium hexametaphosphate 99, tsp, SAP 73 (sodium) (molecular weight 1000～5000), HPMA (molecular weight 400～800), the ZX-I (molecular weight 1000～10000).
Preferably, said 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, said inhibiter is ethylene diamine tetra methylene phosphonic acid sodium (C
6H
12O
12N
2P
4Na
8), HEDP (C
2H
8O
7P
2), ATMP (N (CH
2PO
3H
2)
3), diethylene triamine pentamethylene phosphonic (C
9H
28O
15N
3P
5), one or more the mixture in the polyamino polyether base methylenephosphonic acid (molecular weight about 600, molecular formula is following).
Preferably, said solvent is a deionized water.
The present invention also provides above-mentioned emulsion splitter preparation of compositions method to be: by above-mentioned weight percent emulsion splitter, dispersion agent, permeate agent, inhibiter, solvent are added to vessel in heating (or not heating); After mixing; Be cooled to room temperature, obtain the emulsion splitter composition product.
The present invention also provides the application of above-mentioned emulsion splitter compsn in delayed coking unit.
Preferably, emulsion splitter compsn of the present invention is applicable to that with paraffinic base, intermediate base, naphthenic residual oil be the delayed coking unit of raw material.
The present invention also provides the method for use of above-mentioned emulsion splitter compsn, during use, emulsion splitter is joined after the water cooling plant before the gun barrel, and add-on is the 100-200ppm of coke cooling water.
The beneficial effect that the present invention had:
Emulsion splitter compsn of the present invention mainly contains emulsion splitter, dispersion agent, permeate agent, inhibiter and solvent.Emulsion splitter compsn of the present invention can be realized the fast emulsion breaking of coke cooling water, significantly reduces the oleaginousness in the water; Water body is limpid behind the breakdown of emulsion; Reduce water body to corrosion on Equipment; Do not contain simultaneously mineral ion, existing water body system is not had influence.
Emulsion splitter compsn good water solubility of the present invention can be dissolved each other with sour water fast; Filling is convenient, does not influence the ordinary production of device, does not influence quality product.
Embodiment
Below through embodiment technical scheme of the present invention is described further, but do not limit protection scope of the present invention.
Embodiment 1
A kind of emulsion splitter preparation of compositions method comprises the steps: with 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%), be added to mix in the container after; Be cooled to room temperature, filter and obtain emulsion splitter compsn A product.
Embodiment 2
A kind of emulsion splitter preparation of compositions method comprises the steps: with 250g alkylphenol-formaldehyde resin polyoxyethylene poly-oxygen propylene aether (25%) 200g tsp (20%); 250g propanediol polyoxypropylene polyoxyethylene blocks polyethers (25%); 200g ethylene diamine tetra methylene phosphonic acid sodium (20%), 100g deionized water (10%), be added to mix in the container after; Be cooled to room temperature, filter and obtain emulsion splitter compsn B product.
Embodiment 3
A kind of emulsion splitter preparation of compositions method comprises the steps: with 120g alkylphenol-formaldehyde resin polyoxyethylene poly-oxygen propylene aether (12%) 200g SAP 73 (sodium) (20%); 120g paregal O-15 (12%), 110g HEDP (11%), 450g deionized water (45%); Be added to vessel in heating; After mixing, be cooled to room temperature, filter and obtain emulsion splitter compsn C product.
Embodiment 4
A kind of emulsion splitter preparation of compositions method comprises the steps: with 180g alkylphenol-formaldehyde resin polyoxyethylene polyoxypropylene ether (18%) 180g tsp (18%); 130g propanediol polyoxypropylene polyoxyethylene blocks polyethers (13%); 100g HEDP (10%), 410g deionized water (41%), be added to mix in the container after; Be cooled to room temperature, filter and obtain emulsion splitter compsn D product.
Embodiment 5
A kind of emulsion splitter preparation of compositions method comprises the steps: with 140g alkylphenol-formaldehyde resin polyoxyethylene polyoxypropylene ether (14%) 160g SAP 73 (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 mixing, be cooled to room temperature, filter and obtain emulsion splitter compsn E product.
Embodiment 6
A kind of emulsion splitter preparation of compositions method comprises the steps: with 150g polyethylene polyamine polyoxypropylene propylene ether (15%) 200g HPMA (20%); 110g paregal O-15 (11%), 120g HEDP (12%), 420g deionized water (42%); Be added to vessel in heating; After mixing, be cooled to room temperature, filter and obtain emulsion splitter composition F product.
Embodiment 7
A kind of emulsion splitter preparation of compositions method comprises the steps: with 10g polyethylene polyamine propylene polyethenoxy ether (1%) 10g HPMA (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 mixing, be cooled to room temperature, filter and obtain emulsion splitter compsn G product.
Embodiment 8
A kind of emulsion splitter preparation of compositions method comprises the steps: with 125g polyethylene polyamine polyoxypropylene propylene ether (12.5%) 100g Sodium hexametaphosphate 99 (10%); 125g propanediol polyoxypropylene polyoxyethylene blocks polyethers (12.5%), 100g HEDP (15%), 500g deionized water (50%); Be added to vessel in heating; After mixing, be cooled to room temperature, filter and obtain emulsion splitter compsn H product.
Embodiment 9
A kind of emulsion splitter preparation of compositions method comprises the steps: with 250g alkylphenol-formaldehyde resin polyoxyethylene polyoxypropylene ether (25%) 100g SAP 73 (sodium) (10%); 50g propanediol polyoxypropylene polyoxyethylene blocks polyethers (5%); 150g diethylene triamine pentamethylene phosphonic (15%), 450g deionized water (45%), be added to mix in the container after; Be cooled to room temperature, filter and obtain emulsion splitter composition I product.
Embodiment of the invention 1-9 is the lab scale that the emulsion splitter compsn is used for the effect of delayed coking coke cooling water, with regard to 50ppm, 100ppm, 150ppm, 200ppm difference dosage each product of delayed coking coke cooling water emulsion splitter compsn is made an experiment respectively.
With coke-cooling waste water (fetching water during little feedwater); Carry out quantitative packing, one glass of every 100g water sample, the emulsion splitter compsn with embodiment 1-9 quantitatively is added drop-wise in the beaker that fills coke cooling water by identical dosage respectively; Stir 5min; Rotating speed 350r/min behind the timing 30min, carries out the measurement of water body oleaginousness, COD.The lab scale result sees table 1-4.
Table 1 dosage is the 50ppm test-results
Table 2 dosage is the 100ppm test-results
Table 2 dosage is the 150ppm test-results
Table 3 dosage is the 200ppm test-results
Blank is the control group that does not add the emulsion splitter compsn, can find out that from little test result the oleaginousness along with the emulsion splitter dosage, the removal trend of COD obviously increase, and the effect of taking all factors into consideration the I product is better than other products.
The concrete detection method of oleaginousness, COD:
The COD detection 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, SRM 935a standardized solution, ferrous ammonium sulphate standardized solution, graduated cylinder, zero(ppm) water.
The COD detection method:
In the Erlenmeyer flask of 500ml, add the 0.5g Mercury bisulfate, add liquid to be measured (5ml liquid to be measured adds the distilled water diluting of the 20ml) 25ml after diluting, add vitriol oil 10ml; Shake up; Measure SRM 935a standardized solution 10ml and add in the liquid to be measured for preparing, add sulfuric acid-silver sulfate solution of 40ml again, shake up; After beginning to be heated to boiling, during the add-back flowmeter 5 minutes.
Treat the distilled water flushing prolong of its cooling back, make overall solution volume be no less than 140ml with 100ml.
Solution cools off the back fully and adds 3 phenanthroline ion indicator, uses the ferrous ammonium sulphate standard solution titration, and solution is titration end point by yellow through blue-greenish colour to sorrel, and it is long-pending that record consumes mark liquid.
Step when replacing all the other steps of liquid to be measured after the dilution with test liquid to be measured with 25ml zero(ppm) water when blank is identical.
Calculate: COD=(V
0-V
1) * C * 8 * 1000/V
The volumetric molar concentration (mol/L) of C------ferrous ammonium sulphate standardized solution in the formula
V
0--consume the volume (ml) of ferrous ammonium sulphate when-----titration is blank
V
1Consume the volume (ml) of ferrous ammonium sulphate during-----titration liquid to be measured
The volume of V-------liquid to be measured (ml)
8-------oxygen (1/20) molar mass (g/mol)
Oleaginousness detects: the laboratory apparatus medicine:
The sherwood oil of 60～90 ℃ of boiling points, analytical pure NaCl, water sample to be measured, electronic balance (being accurate to 0.01g), one of 250ml separating funnel, three of small beakers, two in 50ml measuring cup, constant temperature roaster.
The oleaginousness detection method
1. take by weighing 2～3gNaCl with electronic balance and pour separating funnel into, get a beaker again, weighed amount ml, and perform sign.
2. measure 20ml water sample to be measured with measuring cup, pour separating funnel into.
3. get 10～12ml sherwood oil with the another measuring cup and pour separating funnel into.
4. right hand forefinger minor details are withstood funnel upper end glass plug, hold funnel with thumb and forefinger with middle finger again, and left-handed forefinger and middle finger are curled up and be held on the handle of piston, and jolting separating funnel gently up and down makes two fully to contact between mutually, with the raising extraction efficiency.After every jolting several times, will the funnel afterbody be inclined upwardly (towards unmanned place) open the piston venting, to remove the pressure in the funnel.After having only very little pressure when so being repeated to venting, shaken 2～3min leaves standstill again; Treat two mutually fully separately after, open top Bo Sai, again piston is slowly outwarded winding; Lower floor's liquid is emitted from piston, also should put simultaneously at two alternate some flosss that possibly occur sometimes.Then supernatant liquid is poured into the small beaker that weighs up weight from separating funnel is suitable for reading, put into baking box and be baked to and no longer include liquid substance.
5. take by weighing small beaker and solid matter gross weight m2 that baking finishes.
Calculate: oleaginousness (mg/l)=(m2-m1)/v * 106
In the formula: ml and m2 unit are g, v=20ml
The above only is preferred embodiment of the present invention, is not technical scheme of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (10)
1. delayed coking coke cooling water emulsion splitter compsn, it is characterized in that: the component of this emulsion splitter compsn and the mass percentage content of each component are: emulsion splitter 1-25%, dispersion agent 1-20%, permeate agent 1-25%, inhibiter: 1-20%, all the other are solvent.
2. according to the said a kind of delayed coking coke cooling water emulsion splitter compsn of claim 1; It is characterized in that: the component of this emulsion splitter compsn 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. according to claim 1 or 2 said a kind of delayed coking coke cooling water emulsion splitter compsns, it is characterized in that: said 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), the polyethylene polyamine polyoxypropylene propylene ether (AP111, AP126, AP257).
4. according to each said a kind of delayed coking coke cooling water emulsion splitter compsn of claim 1-3, it is characterized in that: said dispersion agent is one or more the mixture in Sodium hexametaphosphate 99, tsp, SAP 73 (sodium) (molecular weight 1000～5000), HPMA (molecular weight 400～800), the ZX-I (molecular weight 1000～10000).
5. according to each said a kind of delayed coking coke cooling water emulsion splitter compsn of claim 1-4, it is characterized in that: said permeate agent is propanediol polyoxypropylene polyoxyethylene blocks polyethers (molecular weight 2000～3000), the paregal O-15 (mixture of one or more of C42～48H86～98O16), Nonyl pheno (12) ether phosphoric acid monoesters.
6. according to each said a kind of delayed coking coke cooling water emulsion splitter compsn of claim 1-5, it is characterized in that: said inhibiter is one or more the mixture in ethylene diamine tetra methylene phosphonic acid sodium, HEDP, ATMP, diethylene triamine pentamethylene phosphonic, the polyamino polyether base methylenephosphonic acid.
7. according to each said a kind of delayed coking coke cooling water emulsion splitter compsn of claim 1-6, it is characterized in that: said solvent is a deionized water.
8. each said emulsion splitter preparation of compositions method of claim 1-7 is: it is characterized in that: emulsion splitter, dispersion agent, permeate agent, inhibiter, solvent are added to vessel in heating or do not heat by above-mentioned weight percent; After mixing; Be cooled to room temperature, obtain the emulsion splitter composition product.
9. each said emulsion splitter compsn application in delayed coking unit of claim 1-7.
10. the method for use of the said emulsion splitter compsn of claim 1-7 is characterized in that: during use, emulsion splitter is joined after the water cooling plant before the gun barrel, add-on is the 100-200ppm of coke cooling water.
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