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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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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