CN104292447A - Coal tar high-efficiency demulsifying agent and preparation method thereof - Google Patents
Coal tar high-efficiency demulsifying agent and preparation method thereof Download PDFInfo
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- CN104292447A CN104292447A CN201410479504.6A CN201410479504A CN104292447A CN 104292447 A CN104292447 A CN 104292447A CN 201410479504 A CN201410479504 A CN 201410479504A CN 104292447 A CN104292447 A CN 104292447A
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- coal tar
- oxyethane
- propylene oxide
- thinner
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- 239000011280 coal tar Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 title abstract description 15
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 238000007599 discharging Methods 0.000 claims abstract description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- 238000012661 block copolymerization Methods 0.000 claims abstract description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003999 initiator Substances 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 239000001294 propane Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 4
- UYMKPFRHYYNDTL-UHFFFAOYSA-N ethenamine Chemical compound NC=C UYMKPFRHYYNDTL-UHFFFAOYSA-N 0.000 claims description 3
- 239000003245 coal Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 abstract 3
- 239000003085 diluting agent Substances 0.000 abstract 3
- 230000000977 initiatory effect Effects 0.000 abstract 3
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000005070 sampling Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000839 emulsion Substances 0.000 description 15
- 239000002994 raw material Substances 0.000 description 14
- 239000003921 oil Substances 0.000 description 12
- 238000009826 distribution Methods 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 239000010779 crude oil Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 108010010803 Gelatin Proteins 0.000 description 2
- 229920001400 block copolymer Polymers 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000010612 desalination reaction Methods 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 239000008273 gelatin Substances 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
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- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to the technical field of coal chemical industry, and aims at providing a coal tar high-efficiency demulsifying agent with good coal tar adaptability and high demulsifying efficiency. The coal tar high-efficiency demulsifying agent comprises the following components in parts by weight: 15-25 parts of epoxy propane, 40-50 parts of epoxy ethane, 0.5-1 part of initiating agent, 24-35 parts of diluting agent and 0-0.6 part of alkali, wherein the initiating agent is isopropanol, glycerol or polyvinylamine, the diluting agent is C9 solvent oil and the alkali is potassium hydroxide or sodium hydroxide. The preparation method of the coal tar high-efficiency demulsifying agent comprises the following steps of: firstly weighing or metering the components in parts by weight; pressing epoxy propane and epoxy ethane into a meter; adding the initiating agent to a reaction kettle, then slowly introducing epoxy ethane and epoxy propane, controlling temperature inside the reaction kettle at 100-200 DEG C, and then carrying out vacuum dehydration for 60 minutes; carrying out block copolymerization under the condition that the pressure is 0.5-0.2 Mpa and the temperature is 130-150 DEG C; after reaction is finished, reducing the pressure inside the reaction kettle to zero, and keeping the temperature for 30 minutes; sampling, assaying a sample to be qualified, then discharging, adding the C9 solvent oil as a diluting agent, uniformly stirring, and then barrelling.
Description
Technical field
The present invention relates to technical field of coal chemical industry, particularly a kind of coal tar high-efficient demulsifier and preparation method thereof.
Background technology
Along with the rise of International Crude Oil, constantly increase with the cost of crude oil for main production vapour, coal, diesel oil, with gelatin liquefaction carry out further hydrocracking produce vapour, coal, diesel oil benefit progressively obvious.But in the production process of coal tar, a large amount of polymer substance (as naphthenic acid, bituminous matter, paraffin) can be produced, these materials can play the effect of emulsifying agent, interfacial film can be formed especially at profit (0-W) interface, this interfacial film has very high viscosity and higher surface tension, to stop droplets form, thus form stable coal tar emulsifying liquid.And the impurity of the coal tar after gelatin liquefaction is more than crude oil, higher, the easy emulsification of acidity, emulsification coal tar are difficult to remove heavy metal and salt, and this will directly affect the carrying out of coal tar subsequent processing, thus affect yield and the quality of product further.Existing emulsion splitter on the market exist low to coal tar bad adaptability, breakdown of emulsion efficiency, easily cause the problems such as corrosion.For this reason, developing a kind of efficient coal tar emulsion splitter is the anxious new technology that must solve of current oil refining industry.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of, coal tar high-efficient demulsifier that breakdown of emulsion efficiency high good to coal tar adaptability and preparation method thereof.
Coal tar high-efficient demulsifier of the present invention, as follows with parts by weight of component:
Propylene oxide 15 ~ 25 parts, 40 ~ 50 parts, oxyethane, initiator 0.5 ~ 1, thinner 24 ~ 35 parts, 0 ~ 0.6 part, alkali; Described initiator is Virahol, glycerol or ethyleneamine, and described thinner is carbon nine solvent oil, and described alkali is potassium hydroxide or sodium hydroxide.
Further, coal tar high-efficient demulsifier of the present invention, as follows with parts by weight of component: described propylene oxide 20 parts, 45 parts, oxyethane, initiator 0.5 part, thinner 35 parts.
Further, coal tar high-efficient demulsifier of the present invention, as follows with parts by weight of component: described propylene oxide 20 parts, 45 parts, oxyethane, initiator 0.5 part, thinner 35 parts, 0.5 part, alkali.
The preparation method of coal tar high-efficient demulsifier of the present invention, comprise following steps: first take according to weight part or measure each component, by alcoxyl propane and oxyethane press-in gauger, initiator is dropped in reactor, then slowly oxyethane is passed into, propylene oxide, temperature in still is controlled after 100 ~ 200 DEG C, vacuum hydro-extraction 60 minutes, at pressure 0.5 ~ 0.2Mpa, block copolymerization is carried out under the condition that temperature is 130 ~ 150 DEG C, after completion of the reaction, still internal pressure is reduced to zero, be incubated 30 minutes, after sample examination is qualified, discharging add carbon nine solvent oil stir as thinner after barrelling.
Further, described oxyethane and propylene oxide at least divide respectively and add for three times, and each add-on of described oxyethane is 13 ~ 17 parts, and each add-on of described propylene oxide is 6 ~ 9 parts.
Further, pressure during described vacuum hydro-extraction is: negative pressure 93100 ~ 98420pa.
Further, during described discharging, temperature is less than 60 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: this emulsion splitter, to coal tar strong adaptability, effectively can abolish the emulsion in coal tar, water droplet is flocculated and coalescent, and rapid subsidence is separated, thus further effective elimination salt and other metal; Can carry out with water filling, injecting and added electric field, effect is more obvious simultaneously; This product can add alkali and regulate pH value, to equipment non-corrosiveness.This preparation method's raw material gradation is stirred and is added, and raw material is mixed more even, and this feed postition makes oxyethane and propylene oxide tentatively crosslinked, subsequent polymerisation reaction does not need to use linking agent, and the block copolymer distribution that polyreaction is produced is more even; First dewater before raw material reaction, incite somebody to action wherein moisture removal, be conducive to follow-up polyreaction.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment one
Coal tar high-efficient demulsifier of the present invention, as follows with parts by weight of component:
Propylene oxide 25 parts, 40 parts, oxyethane, initiator 1, thinner 24 parts; Described initiator is Virahol, and described thinner is carbon nine solvent oil.
This emulsion splitter preparation method comprises following steps: first take according to weight part or measure each component, by alcoxyl propane and oxyethane press-in gauger, initiator is dropped in reactor, then slowly oxyethane is passed into, propylene oxide, temperature in still is controlled after 100 ~ 200 DEG C, vacuum and negative pressure 93100 ~ 98420pa dewater 60 minutes, at pressure 0.5 ~ 0.2Mpa, block copolymerization is carried out under the condition that temperature is 130 ~ 150 DEG C, after completion of the reaction, still internal pressure is reduced to zero, be incubated 30 minutes, make reaction more abundant, after sample examination is qualified, discharging add carbon nine solvent oil stir as thinner after barrelling.Wherein, during discharging, temperature is less than 60 DEG C.
Wherein, described oxyethane and propylene oxide divide three times respectively and add, and are specially, and in reactor, first pass into the oxyethane of 14 parts, then pass into the propylene oxide of 9 parts, stir; In reactor, again pass into the oxyethane of 13 parts, then pass into the propylene oxide of 8 parts, stir; For the third time, in reactor, pass into the oxyethane of 13 parts, then pass into the propylene oxide of 8 parts, stir.It is more even that the raw material mode that gradation adds under agitation makes raw material mix, and this feed postition makes oxyethane and propylene oxide tentatively crosslinked, subsequent polymerisation reaction does not need to use linking agent, when being conducive to follow-up segmented copolymer, and the homogeneity of products distribution.
Embodiment two
Coal tar high-efficient demulsifier of the present invention, as follows with parts by weight of component: propylene oxide 20 parts, 45 parts, oxyethane, initiator 0.5, thinner 35 parts; Described initiator is ethyleneamine, and described thinner is carbon nine solvent oil.
This emulsion splitter preparation method comprises following steps: first take according to weight part or measure each component, by alcoxyl propane and oxyethane press-in gauger, initiator is dropped in reactor, then slowly oxyethane is passed into, propylene oxide, temperature in still is controlled after 100 ~ 200 DEG C, vacuum and negative pressure 93100 ~ 98420pa dewater 60 minutes, at pressure 0.5 ~ 0.2Mpa, block copolymerization is carried out under the condition that temperature is 130 ~ 150 DEG C, after completion of the reaction, still internal pressure is reduced to zero, be incubated 30 minutes, make reaction more abundant, after sample examination is qualified, discharging add carbon nine solvent oil stir as thinner after barrelling.Wherein, during discharging, temperature is less than 60 DEG C.
Wherein, described oxyethane and propylene oxide divide three times respectively and add, and are specially, and in reactor, first pass into the oxyethane of 15 parts, then pass into the propylene oxide of 7 parts, stir; In reactor, again pass into the oxyethane of 15 parts, then pass into the propylene oxide of 7 parts, stir; For the third time, in reactor, pass into the oxyethane of 15 parts, then pass into the propylene oxide of 6 parts, stir.It is more even that the raw material mode that gradation adds under agitation makes raw material mix, and this feed postition makes oxyethane and propylene oxide tentatively crosslinked, subsequent polymerisation reaction does not need to use linking agent, when being conducive to follow-up segmented copolymer, and the homogeneity of products distribution.
Embodiment three
Coal tar high-efficient demulsifier of the present invention, is formulated as with weight part: propylene oxide 20 parts, 45 parts, oxyethane, initiator 0.5, thinner 35 parts, 0.5 part, alkali; Described initiator is glycerol, and described thinner is carbon nine solvent oil, and described alkali is potassium hydroxide.
This emulsion splitter preparation method comprises following steps: first take according to weight part or measure each component, by alcoxyl propane and oxyethane press-in gauger, initiator is dropped in reactor, then slowly oxyethane is passed into, propylene oxide, temperature in still is controlled after 100 ~ 200 DEG C, vacuum and negative pressure 93100 ~ 98420pa dewater 60 minutes, at pressure 0.5 ~ 0.2Mpa, block copolymerization is carried out under the condition that temperature is 130 ~ 150 DEG C, after completion of the reaction, still internal pressure is reduced to zero, be incubated 30 minutes, make reaction more abundant, after sample examination is qualified, discharging add carbon nine solvent oil stir as thinner after barrelling.Wherein, during discharging, temperature is less than 60 DEG C.
Wherein, described oxyethane and propylene oxide divide three times respectively and add, and are specially, and in reactor, first pass into the oxyethane of 15 parts, then pass into the propylene oxide of 7 parts, stir; In reactor, again pass into the oxyethane of 15 parts, then pass into the propylene oxide of 7 parts, stir; For the third time, in reactor, pass into the oxyethane of 15 parts, then pass into the propylene oxide of 6 parts, stir.It is more even that the raw material mode that gradation adds under agitation makes raw material mix, and this feed postition makes oxyethane and propylene oxide tentatively crosslinked, subsequent polymerisation reaction does not need to use linking agent, when being conducive to follow-up segmented copolymer, and the homogeneity of products distribution.
Add alkali in coal tar high-efficient demulsifier of the present invention and can play the effect preventing etching apparatus.
Embodiment four
Coal tar high-efficient demulsifier of the present invention, is formulated as with weight part: propylene oxide 15 parts, 50 parts, oxyethane, initiator 0.8 part, thinner 30 parts; Described initiator is glycerol, and described thinner is carbon nine solvent oil.
This emulsion splitter preparation method comprises following steps: first take according to weight part or measure each component, by alcoxyl propane and oxyethane press-in gauger, initiator is dropped in reactor, then slowly oxyethane is passed into, propylene oxide, temperature in still is controlled after 100 ~ 200 DEG C, vacuum and negative pressure 93100 ~ 98420pa dewater 60 minutes, at pressure 0.5 ~ 0.2Mpa, block copolymerization is carried out under the condition that temperature is 130 ~ 150 DEG C, after completion of the reaction, still internal pressure is reduced to zero, be incubated 30 minutes, make reaction more abundant, after sample examination is qualified, discharging add carbon nine solvent oil stir as thinner after barrelling.Wherein, during discharging, temperature is less than 60 DEG C.
Wherein, described oxyethane and propylene oxide divide three times respectively and add, and are specially, and in reactor, first pass into the oxyethane of 20 parts, then pass into the propylene oxide of 5 parts, stir; In reactor, again pass into the oxyethane of 15 parts, then pass into the propylene oxide of 5 parts, stir; For the third time, in reactor, pass into the oxyethane of 15 parts, then pass into the propylene oxide of 5 parts, stir.It is more even that the raw material mode that gradation adds under agitation makes raw material mix, and this feed postition makes oxyethane and propylene oxide tentatively crosslinked, subsequent polymerisation reaction does not need to use linking agent, when being conducive to follow-up segmented copolymer, and the homogeneity of products distribution.
Coal tar high-efficient demulsifier of the present invention, to coal tar strong adaptability, effectively can abolish the emulsion in coal tar, water droplet is flocculated and coalescent, and rapid subsidence is separated, thus further effective elimination salt and other metal; Can carry out with water filling, injecting and added electric field, effect is more obvious simultaneously; Do not affect next procedure; This product can add alkali and regulate pH value, to equipment non-corrosiveness.
Coal tar high-efficient demulsifier of the present invention, generally injected before coal tar desalination, its injection rate is 2/1000000ths ten to five ten, namely 20 ~ 50 tons of these emulsion splitters to be added inside 1,000,000 tons of coal tar emulsifying liquid, adopt continuous injection mode, can inject with desalting agent, decalcifying agent simultaneously, need before entering desalter to increase static mixer, so that various doses mix with coal tar; This emulsion splitter toxicological harmless itself, but skin, eyes, oral cavity can not be contacted, want timely clear water to rinse well as touched.Through experimental test result, after adding this emulsion splitter, emulsion can 98% to be abolished, and it is clear that water-oil interface are separated, and desalination decalcification effect is good, can meet the pretreated processing requirement of coal tar.
The preparation method of coal tar high-efficient demulsifier of the present invention, raw material gradation is stirred and is added, raw material is mixed more even, and this feed postition makes oxyethane and propylene oxide tentatively crosslinked, subsequent polymerisation reaction does not need to use linking agent, and the block copolymer distribution that polyreaction is produced is more even; First dewater before raw material reaction, incite somebody to action wherein moisture removal, be conducive to follow-up polyreaction.
Comprise the above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (7)
1. a coal tar high-efficient demulsifier, is characterized in that, as follows with parts by weight of component:
Propylene oxide 15 ~ 25 parts, 40 ~ 50 parts, oxyethane, initiator 0.5 ~ 1, thinner 24 ~ 35 parts, 0 ~ 0.6 part, alkali; Described initiator is Virahol, glycerol or ethyleneamine, and described thinner is carbon nine solvent oil, and described alkali is potassium hydroxide or sodium hydroxide.
2. coal tar high-efficient demulsifier as claimed in claim 1, is characterized in that, as follows with parts by weight of component: described propylene oxide 20 parts, 45 parts, oxyethane, initiator 0.5, thinner 35 parts.
3. coal tar high-efficient demulsifier as claimed in claim 1, is characterized in that, as follows with parts by weight of component: described propylene oxide 20 parts, 45 parts, oxyethane, initiator 0.5 part, thinner 35 parts, 0.5 part, alkali.
4. the preparation method of coal tar high-efficient demulsifier as claimed in claim 1, it is characterized in that, comprise following steps: first take according to weight part or measure each component, by alcoxyl propane and oxyethane press-in gauger, initiator is dropped in reactor, then slowly oxyethane is passed into, propylene oxide, temperature in still is controlled after 100 ~ 200 DEG C, vacuum hydro-extraction 60 minutes, at pressure 0.5 ~ 0.2Mpa, block copolymerization is carried out under the condition that temperature is 130 ~ 150 DEG C, after completion of the reaction, still internal pressure is reduced to zero, be incubated 30 minutes, after sample examination is qualified, discharging add carbon nine solvent oil stir as thinner after barrelling.
5. coal tar high-efficient demulsifier as claimed in claim 4, it is characterized in that, described oxyethane and propylene oxide at least divide respectively and add for three times, and each add-on of described oxyethane is 13 ~ 17 parts, and each add-on of described propylene oxide is 6 ~ 9 parts.
6. coal tar high-efficient demulsifier as claimed in claim 4, it is characterized in that, pressure during described vacuum hydro-extraction is: negative pressure 93100 ~ 98420pa.
7. coal tar high-efficient demulsifier as claimed in claim 4, it is characterized in that, during described discharging, temperature is less than 60 DEG C.
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CN201410479504.6A CN104292447A (en) | 2014-09-18 | 2014-09-18 | Coal tar high-efficiency demulsifying agent and preparation method thereof |
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CN201410479504.6A CN104292447A (en) | 2014-09-18 | 2014-09-18 | Coal tar high-efficiency demulsifying agent and preparation method thereof |
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CN107868241A (en) * | 2017-11-24 | 2018-04-03 | 威海翔泽新材料科技有限公司 | A kind of fatty alcohol block polyether class tar ammonia demulsifier and preparation method thereof |
CN108276571A (en) * | 2017-12-25 | 2018-07-13 | 威海翔泽新材料科技有限公司 | A kind of preparation of the dedicated efficient dehydration of tar agent of coking of coal |
CN114292664A (en) * | 2021-12-28 | 2022-04-08 | 江苏汉光实业股份有限公司 | Oil-soluble demulsifying desalting agent and preparation method thereof |
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CN114292664A (en) * | 2021-12-28 | 2022-04-08 | 江苏汉光实业股份有限公司 | Oil-soluble demulsifying desalting agent and preparation method thereof |
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