CN102585885B - Method for re-purifying and recovering liquid paraffin obtained after solvent extraction - Google Patents
Method for re-purifying and recovering liquid paraffin obtained after solvent extraction Download PDFInfo
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- CN102585885B CN102585885B CN201210003828.3A CN201210003828A CN102585885B CN 102585885 B CN102585885 B CN 102585885B CN 201210003828 A CN201210003828 A CN 201210003828A CN 102585885 B CN102585885 B CN 102585885B
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Abstract
The invention provides a method for re-purifying and recovering liquid paraffin obtained after solvent extraction. By the recovery method, the liquid paraffin recovered after solvent extraction is performed and the solvent is removed is re-purified. The method mainly comprises the steps of acid washing, neutralizing, washing and settling; impurities such as inorganic salt, gelatin, and surfactant are removed, the heavy-component proportion of the obtained high-purity liquid paraffin is basically consistent with that of the unused industrial liquid paraffin, and the high-purity liquid paraffin can be applied to polymerization reaction of a macroporous ion exchange resin again. The technical scheme has the technical characteristics of simple and short process, and high purification rate.
Description
Technical field
The recovery method of the waste liq paraffin that what patent application of the present invention related to is produces in macroreticular ion exchange resin preparation technology, the in particular method of purification again of the whiteruss after solvent extraction.
Background technology
Whiteruss is widely used, relate to every field, it is the normal paraffin being made up of 11～18 carbon atoms in a kind of molecule, in ion exchange resin manufacturing process, whiteruss, mainly as the pore-creating agent of polymkeric substance, is one of conventional raw material of preparing macroreticular ion exchange resin.After polyreaction completes, common solvent extraction process recovering liquid paraffin, then manage to remove solvent wherein.Prior art also provides a kind of method of Distillation recovery whiteruss, as adopted distillation method recovering liquid paraffin under 210～320 ℃ of temperature condition in the patent No. Chinese patent technology that is 200410012202.4, but this separation method exists the technical problem that energy consumption is high, particularly whiteruss under distillation high temperature, to there will be the technical problem of oxidation stain.
Adopt solvent extration recovering liquid paraffin, the whiteruss obtaining through removing solvent process again, wherein contain water, tensio-active agent, gelatin, the impurity such as low-molecular-weight polystyrene, these impurity all come from dispersion agent and the dispersion aids that in polymerization process, water adds, as gelatin, magnesiumcarbonate, methylene blue etc., and the polystyrene of polymerization stage formation, lower molecular weight line style or the three-dimensional polymers such as poly-divinylbenzene, the whiteruss obtaining through above-mentioned recovery method is re-used as pore-creating agent reuse to the polyreaction of macroreticular ion exchange resin, the impurity that whiteruss contains will affect the epigranular degree of polymerisate, reduce the ultimate compression strength of spheroid and occur aspherical particle.Therefore reclaim and remove whiteruss that solvent obtains by solvent extraction and be the pore-creating agent application that is difficult to be re-used as macroreticular ion exchange resin polymerization reaction zone.
Summary of the invention
The goal of the invention of patent application of the present invention is by solvent extraction and after removing solvent to reclaim purify the again recovery method of purifying again of the liquid paraffin obtained after solvent extraction that makes high purity whiteruss of the whiteruss obtaining, and the recovery method of purifying again of this liquid paraffin obtained after solvent extraction has realized that the whiteruss that makes is can direct reuse simple to macroreticular ion exchange resin polymerization process and technique, the technical purpose of less energy-consumption.The recovery method technical scheme of purifying again of the liquid paraffin obtained after solvent extraction that patent application of the present invention provides, its main technical content is: a kind of recovery method of purifying again of liquid paraffin obtained after solvent extraction, this recovery method is to solvent extraction and after removing solvent, reclaims the purification processing method again of the whiteruss obtaining, be intermediate liquid paraffin hereinafter referred to as this whiteruss, present method mainly includes pickling, neutralization, washing and four processing steps of sedimentation: 1. pickling: under room temperature condition, start the reactor agitator that intermediate liquid paraffin is housed, stirring velocity is not less than 60 turn/min, be 70～98% sulfuric acid to slowly adding concentration in reactor, sulfuric acid consumption is 8～10% of intermediate liquid Quality of Paraffin Waxes, add after sulfuric acid, stir 30min, then leave standstill 5～12h, the lower floor's acid sludge liquid of draining, upper strata liquid is treated 2. step processing, and inorganic salt, gelatin, tensio-active agent etc. enter the acid sludge layer of lower floor in this stage, removed by layering.2. neutralization: 1. walking upper strata liquid to the in stirring, to add concentration be 1～3% soda ash or aqueous sodium hydroxide solution, in and remaining sulfuric acid in the liquid of upper strata, make pH value reach neutrality, then after stratification, subnatant discharged; 3. washing: 2. walk to that to add pure water, amount of water in the liquid of upper strata be middle, stir and wash, get rid of lower floor's waste liquid after stratification; 4., sedimentation: the intermediate liquid paraffin after washing is sent into plate separator sedimentation, and solid oligomer sedimentation is drained, and obtains high purity whiteruss.In the acid pickling step of the technical program, slowly adding sulfuric acid is to occur local superheating phenomenon in sulfuric acid adition process, and this sulfuric acid can be answered the Waste Sulfuric Acid producing in spent ion exchange resin preparation process.
In above-mentioned overall technical architecture, the amount of water of washing is preferably 0.2-1 times of whiteruss quality, if plant capacity allows, passable in more amount of water, but the one, can waste water, the 2nd, understand a small amount of dissolution fluid paraffin body, increase the pressure of later stage water treatment.
The advantage of the recovery method of purifying again of the liquid paraffin obtained after solvent extraction of patent application of the present invention is: 1, this recovery method has advantages of less energy-consumption, without heating or distillation for processing; 2, the sulfuric acid in pickling can be answered the Waste Sulfuric Acid producing in spent ion exchange resin production process, remove the acid-soluble impurity in whiteruss, as inorganic salt, gelatin, tensio-active agent etc., the recovery method of refuse reclamation has advantages of that cost is low and meets environmental protection; 3, the technical program technical process is simple, flow process is short, purification rate is high; The weight component ratio of the whiteruss 4, finally obtaining and untapped industrial liquid paraffin are basically identical, can again be applied in the polyreaction of macroreticular ion exchange resin.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of patent application of the present invention
Fig. 2 is the gas chromatogram of industrial liquid paraffin
Fig. 3 is the gas chromatogram of the whiteruss after the present invention reclaims.
Embodiment
To describe technical scheme of the present invention in detail by the embodiment providing below.
Get 1000kg intermediate liquid paraffin, joining volume is in 2000L reactor 1, start whipping appts, revolution is adjusted into 60 turn/min, and slowly adding concentration is 80% Waste Sulfuric Acid 90kg, and this Waste Sulfuric Acid is the Waste Sulfuric Acid producing in ion exchange resin preparation process, certainly more can use industrial sulphuric acid, stir 30min, shut down leave standstill 5h occur upper and lower two-layer after, lower floor's acid solution is drained into waste water neutralization tank 2; Thereafter stir, to the sodium carbonate solution or the sodium hydroxide solution that add 2% in reactor, and finally to adjust pH value be 7 o'clock again, and N-process finishes, and standing 1h forms after upper and lower layering liquid, and a small amount of residual liquid discharge of lower floor is to waste water neutralization tank 2; In reactor, add 200kg pure water, stir 0.5h with the rotating speed that is not less than 60 turn/min, after stratification, lower floor's waste water drains into waste water neutralization tank 2, so once washes again.The waste water producing in pickling, neutralization and water washing process should pass through water treatment operation, just can enter urban sewage treatment system, otherwise can cause two degree water pollutions after waste water neutralization tank 2 neutralizing treatment.Solution in reactor is sent in plate separator 3 and implemented precipitate and separate, the polymkeric substance sedimentation of lower floor is discharged, what the outlet output of separator upper strata obtained is refining whiteruss, sends into whiteruss receiving tank 4.Use 9710 gas chromatographs, adopt 30m × 0.32mm × 0.5 μ m SE-50 type capillary chromatographic column, it is 280 ℃ that sampler temperature, post case temperature, detector temperature are set, sample size is 0.1 μ L, the whiteruss respectively industrial liquid paraffin and the inventive method being obtained carries out gas chromatographic analysis, as shown in Figures 2 and 3, the whiteruss that the inventive method obtains and industrial liquid paraffin are basically identical for gas chromatogram.
Claims (4)
1. the recovery method of purifying again of a liquid paraffin obtained after solvent extraction, this recovery method is to solvent extraction and after removing solvent, reclaims the purification processing method again of the whiteruss obtaining, be intermediate liquid paraffin hereinafter referred to as this whiteruss, it is characterized in that present method mainly includes pickling, neutralization, washing and four processing steps of sedimentation: 1. pickling: under room temperature condition, start the reactor agitator that intermediate liquid paraffin is housed, stirring velocity is not less than 60 turn/min, be 70～98% sulfuric acid to slowly adding concentration in reactor, sulfuric acid consumption is 8～10% of intermediate liquid Quality of Paraffin Waxes, add after sulfuric acid, stir 30min, then leave standstill 5～12h, the lower floor's acid sludge liquid of draining, upper strata liquid is treated 2. step processing, 2. neutralization: 1. walking upper strata liquid to the in stirring, to add concentration be 1～3% soda ash or aqueous sodium hydroxide solution, in and remaining sulfuric acid in the liquid of upper strata, make pH value reach neutrality, then after stratification, subnatant discharged, 3. washing: 2. walk to that to add pure water, amount of water in the liquid of upper strata be middle, stir and wash, get rid of lower floor's waste liquid after stratification, 4., sedimentation: the intermediate liquid paraffin after washing is sent into plate separator sedimentation, and solid oligomer sedimentation is drained, and obtains high purity whiteruss.
2. the recovery method of purifying again of liquid paraffin obtained after solvent extraction according to claim 1, the amount of water that it is characterized in that washing is 0.2-1 times of whiteruss quality.
3. the recovery method of purifying again of liquid paraffin obtained after solvent extraction according to claim 1, the amount of water that it is characterized in that washing is 0.2 times of whiteruss quality, carries out twice washing.
4. the recovery method of purifying again of liquid paraffin obtained after solvent extraction according to claim 1, is characterized in that pickling sulfuric acid is the Waste Sulfuric Acid producing in ion exchange resin preparation process.
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| CN201210003828.3A CN102585885B (en) | 2012-01-08 | 2012-01-08 | Method for re-purifying and recovering liquid paraffin obtained after solvent extraction |
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| CN201210003828.3A CN102585885B (en) | 2012-01-08 | 2012-01-08 | Method for re-purifying and recovering liquid paraffin obtained after solvent extraction |
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| CN102585885A CN102585885A (en) | 2012-07-18 |
| CN102585885B true CN102585885B (en) | 2014-05-21 |
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| CN102888245B (en) * | 2012-09-19 | 2014-07-16 | 沁阳市海世鸿工贸有限责任公司 | Method and device for refining liquid paraffin |
| CN109054077B (en) * | 2018-09-20 | 2021-03-23 | 扬州金珠树脂有限公司 | Method for recycling macroporous ion exchange resin pore-foaming agent |
| CN116463146A (en) * | 2022-01-12 | 2023-07-21 | 中昊晨光化工研究院有限公司 | Paraffin circulating device system and paraffin circulating process for polymer production |
| CN114874810B (en) * | 2022-04-28 | 2024-04-12 | 海南汉地阳光石油化工有限公司 | 60N white oil agent for artificial fiber and preparation method thereof |
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| SU887623A1 (en) * | 1979-08-06 | 1981-12-07 | Московский Ордена Трудового Красного Знамени Институт Нефтехимической И Газовой Промышленности Им. И.М.Губкина | Method of producing liquid paraffins |
| CN1219569C (en) * | 2004-03-19 | 2005-09-21 | 中国科学院山西煤炭化学研究所 | Method of separating and reclaiming spent cobalt based catalyst and heavy hydrocarbon throuth Fishcher-Tropsch synthesis in slurry bed |
| CN102120935B (en) * | 2011-01-10 | 2014-06-04 | 佛山汉维机电科技有限公司 | Method for recycling heptane and saxol from waste saxol containing heptane |
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Non-Patent Citations (4)
| Title |
|---|
| "废旧液体石蜡的回收与再生";赵哲勋;《天津化工》;19900131(第1期);第32-33页 * |
| "废液压油的再生";田树正;《木材加工机械》;19931001(第3期);第15-17页 * |
| 田树正."废液压油的再生".《木材加工机械》.1993,(第3期),第15~17页. |
| 赵哲勋."废旧液体石蜡的回收与再生".《天津化工》.1990,(第1期),第32-33页. |
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