CN102585885A - 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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- CN102585885A CN102585885A CN2012100038283A CN201210003828A CN102585885A CN 102585885 A CN102585885 A CN 102585885A CN 2012100038283 A CN2012100038283 A CN 2012100038283A CN 201210003828 A CN201210003828 A CN 201210003828A CN 102585885 A CN102585885 A CN 102585885A
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- whiteruss
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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
Patented claim of the present invention relates to is the recovery method of the waste liq paraffin that produces among the macroreticular ion exchange resin preparation technology, in particular the method for purification again of the whiteruss after SX.
Background technology
Whiteruss is widely used; Relate to every field, it is the normal paraffin that a kind of intramolecularly is made up of 11～18 carbon atoms, in the ion exchange resin ME; Whiteruss is one of raw material commonly used of preparation macroreticular ion exchange resin mainly as the pore-creating agent of polymkeric substance.After polyreaction was accomplished, common solvent extraction process recovering liq paraffin managed to remove solvent wherein again.Prior art also provides a kind of method of distilling recovering liq paraffin; Be to have adopted distillation method recovering liq paraffin under 210～320 ℃ of temperature condition in 200410012202.4 the Chinese patent technology like the patent No.; But this separation method exists energy consumption high technical problem, particularly whiteruss the technical problem of oxidation stain under distillation high temperature, can occur.
Adopt solvent extration recovering liq paraffin; Again through removing the whiteruss that solvent process obtains; Wherein contain impurity such as water, tensio-active agent, gelatin, low-molecular-weight polystyrene; These impurity all come from dispersion agent and the dispersion aids that water adds in the polymerization process; Like gelatin, magnesiumcarbonate, methylene blue etc.; And the PS that forms of polymerization stage, gather lower molecular weight line style or three-dimensional polymer such as divinylbenzene, remake in the polyreaction into pore-creating agent reuse to macroreticular ion exchange resin through the whiteruss that above-mentioned recovery method obtains, the impurity that whiteruss contains will influence polymerisate epigranular degree, reduction spheroid ultimate compression strength and aspherical particle appears.Therefore the whiteruss that is obtained by SX recovery and removal solvent is that the pore-creating agent that is difficult to remake to the macroreticular ion exchange resin polymerization reaction zone is used.
Summary of the invention
The goal of the invention of patented claim of the present invention is SX and reclaims purify the again recovery method of purification again of the SX whiteruss that makes the high purity whiteruss of the whiteruss obtain after removing solvent, and the whiteruss that the recovery method of purifying again of this SX whiteruss has been realized making can direct reuse to macroreticular ion exchange resin polymerization process and technology is simple, the technical purpose of less energy-consumption.The recovery method of the purification again technical scheme of the SX whiteruss that patented claim of the present invention provides, its major technique content is: a kind of recovery method of purification again of SX whiteruss, this recovery method are the purification processing methods again that reclaims the whiteruss that obtains to SX and after removing solvent; To call this whiteruss in the following text is intermediate liquid paraffin; Present method mainly includes pickling, neutralization, washing and four process steps of sedimentation: 1. pickling: under the room temperature condition, start the reaction kettle whisking appliance that intermediate liquid paraffin is housed, stirring velocity is not less than 60 commentaries on classics/min; In reaction kettle, slowly adding concentration is 70～98% sulfuric acid; The sulfuric acid consumption is 8～10% of an intermediate liquid paraffin quality, add sulfuric acid after, stir 30min; Leave standstill 5～12h then, 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. are removed by layering at the acid sludge layer of this stage entering lower floor.2. neutralization: 1. going on foot upper strata liquid to the in the stirring, to add concentration be 1～3% soda ash or aqueous sodium hydroxide solution, in upper strata liquid in remaining sulfuric acid, make pH value reach neutrality, behind the standing demix, subnatant is discharged again; 3. washing: 2. go on foot to the and to add pure water in the liquid of upper strata, amount of water be middle, stirs washing, eliminating lower floor waste liquid behind the standing demix; 4., sedimentation: the intermediate liquid paraffin after the washing is sent into the plate separator sedimentation, and the solid oligomer sedimentation is drained, and obtains the high purity whiteruss.In the acid pickling step of present technique scheme, slowly adding sulfuric acid is in the sulfuric acid adition process, the local superheating phenomenon to occur, and this sulfuric acid can prepare the sulfur waste acid that produces in the process by the Application of ion exchange resin.
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 the more amount of water; But the one, can waste water, the 2nd, understand a small amount of dissolution fluid paraffin body, increased the pressure of later stage water treatment.
The advantage of the recovery method of purifying again of the SX whiteruss of patented claim of the present invention is: 1, this recovery method has the advantage of less energy-consumption, does not have heating or distillation for processing; 2, the sulfur waste acid that produces in can Application of ion exchange resin production process of the sulfuric acid in the pickling; Remove the solubility in acid impurity in the whiteruss; Like inorganic salt, gelatin, tensio-active agent etc., it is low and meet the advantage of environmental protection that the recovery method of refuse reclamation has a cost; 3, the technical process of present technique scheme is simple, flow process is short, purification rate is high; The weight component ratio of the whiteruss that 4, finally obtains and untapped industrial liquid paraffin basically identical can be applied in the polyreaction of macroreticular ion exchange resin again.
Description of drawings
Fig. 1 is the process flow sheet of patented claim 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 specify technical scheme of the present invention through the embodiment that provides below.
Get 1000kg intermediate liquid paraffin, joining volume is in the 2000L reaction kettle 1, starts whipping appts; Revolution is adjusted into 60 commentaries on classics/min, slowly adds concentration and be 80% sulfur waste acid 90kg, the sulfur waste acid that this sulfur waste acid produces in the process for ion exchange resin prepares; 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 restir adds 2% sodium carbonate solution or sodium hydroxide solution in reaction kettle, and finally to adjust pH value be 7 o'clock, and the N-process end is left standstill after 1h forms upper and lower layering liquid, and a spot of residual liquid discharge of lower floor is to waste water neutralization tank 2; In reaction kettle, add the 200kg pure water, stir 0.5h with the rotating speed that is not less than 60 commentaries on classics/min, behind the standing demix, lower floor's waste water drains into waste water neutralization tank 2, so once washes again.The waste water that produces in pickling, neutralization and the water washing process should pass through the water treatment operation, after waste water neutralization tank 2 neutralizing treatment, just can enter urban sewage treatment system, otherwise can cause two degree water pollutions.Solution in the reaction kettle sent in the plate separator 3 implement precipitate and separate, the polymkeric substance sedimentation of lower floor is discharged, what the outlet output of separator upper strata obtained is the purified 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 oven temperature, degree, detector temperature are set, and sample size is 0.1 μ L, and the whiteruss that respectively industrial liquid paraffin and the inventive method is obtained carries out gas chromatographic analysis; Gas chromatogram as shown in Figures 2 and 3, whiteruss that the inventive method obtains and industrial liquid paraffin basically identical.
Claims (4)
1. the recovery method of purification again of a SX whiteruss, this recovery method are the purification processing methods again that reclaims the whiteruss that obtains to SX and after removing solvent, are intermediate liquid paraffin to call this whiteruss in the following text; It is characterized in that present method mainly includes pickling, neutralization, washing and four process steps of sedimentation: 1. pickling: under the room temperature condition; Start the reaction kettle whisking appliance that intermediate liquid paraffin is housed, stirring velocity is not less than 60 commentaries on classics/min, and in reaction kettle, slowly adding concentration is 70～98% sulfuric acid; The sulfuric acid consumption is 8～10% of an intermediate liquid paraffin quality; After adding sulfuric acid, stir 30min, leave standstill 5～12h then; The lower floor's acid sludge liquid of draining, upper strata liquid treat the, and 2. the step handles; 2. neutralization: 1. going on foot upper strata liquid to the in the stirring, to add concentration be 1～3% soda ash or aqueous sodium hydroxide solution, in upper strata liquid in remaining sulfuric acid, make pH value reach neutrality, behind the standing demix, subnatant is discharged again; 3. washing: 2. go on foot to the and to add pure water in the liquid of upper strata, amount of water be middle, stirs washing, eliminating lower floor waste liquid behind the standing demix; 4., sedimentation: the intermediate liquid paraffin after the washing is sent into the plate separator sedimentation, and the solid oligomer sedimentation is drained, and obtains the high purity whiteruss.
2. the recovery method of purification again of SX whiteruss according to claim 1 is characterized in that the amount of water of washing is 0.2-1 a times of whiteruss quality.
3. the recovery method of purification again of SX whiteruss according to claim 1 is characterized in that the amount of water of washing is 0.2 times of whiteruss quality, carries out twice washing.
4. the recovery method of purification again of SX whiteruss according to claim 1, it is sour to it is characterized in that pickling uses sulfuric acid to prepare the sulfur waste that produces in the process as ion exchange resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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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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| Application Number | Priority Date | Filing Date | Title |
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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 true CN102585885A (en) | 2012-07-18 |
| CN102585885B CN102585885B (en) | 2014-05-21 |
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| CN201210003828.3A Expired - Fee Related CN102585885B (en) | 2012-01-08 | 2012-01-08 | Method for re-purifying and recovering liquid paraffin obtained after solvent extraction |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102888245A (en) * | 2012-09-19 | 2013-01-23 | 沁阳市海世鸿工贸有限责任公司 | Method and device for refining liquid paraffin |
| CN109054077A (en) * | 2018-09-20 | 2018-12-21 | 扬州金珠树脂有限公司 | A kind of reuse method of macroreticular ion exchange resin pore-foaming agent |
| CN114874810A (en) * | 2022-04-28 | 2022-08-09 | 海南汉地阳光石油化工有限公司 | 60N white oil agent for artificial fibers and preparation method thereof |
| 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 |
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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 |
| CN1563280A (en) * | 2004-03-19 | 2005-01-12 | 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 |
| CN102120935A (en) * | 2011-01-10 | 2011-07-13 | 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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2012
- 2012-01-08 CN CN201210003828.3A patent/CN102585885B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN1563280A (en) * | 2004-03-19 | 2005-01-12 | 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 |
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Non-Patent Citations (4)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102888245A (en) * | 2012-09-19 | 2013-01-23 | 沁阳市海世鸿工贸有限责任公司 | Method and device for refining liquid paraffin |
| 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 |
| CN109054077A (en) * | 2018-09-20 | 2018-12-21 | 扬州金珠树脂有限公司 | A kind of reuse method of macroreticular ion exchange resin pore-foaming agent |
| 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 |
| CN114874810A (en) * | 2022-04-28 | 2022-08-09 | 海南汉地阳光石油化工有限公司 | 60N white oil agent for artificial fibers and preparation method thereof |
| 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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| CN102585885B (en) | 2014-05-21 |
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