CN103787820A - Method for recovering toluene from mother liquor for producing polypropylene nucleating agent - Google Patents
Method for recovering toluene from mother liquor for producing polypropylene nucleating agent Download PDFInfo
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- CN103787820A CN103787820A CN201210429978.0A CN201210429978A CN103787820A CN 103787820 A CN103787820 A CN 103787820A CN 201210429978 A CN201210429978 A CN 201210429978A CN 103787820 A CN103787820 A CN 103787820A
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Abstract
The invention provides a method for recovering toluene from mother liquor for producing polypropylene nucleating agents. The method comprises the following steps: firstly performing solid-liquid separation by suction filtration and centrifugal separation of polypropylene nucleating agent reaction mother liquor, allowing the filtrate to stand for layering, discharging the water phase at the lower layer, distilling the oil phase at the upper layer at a normal pressure or reduced pressure condition, and then performing condensation and drying to obtain the purified toluene. The method of the invention significantly reduces the steam consumption, and thus reaches the purposes of energy saving and environmental protection.
Description
Technical field
The present invention relates to organic chemical industry field, particularly relate to the recovery method of mother liquor toluene in a kind of polypropylene nucleater production process.
Background technology
In the process of certain class polypropylene nucleater of preparation, often produce a large amount of reaction mother liquors, the main component in mother liquor is intermediates and some salt of toluene, water, nucleator.Wherein, toluene is that solvent is present in mother liquor in a large number, for reducing production costs and reducing environmental pollution, need recycle the toluene in reaction mother liquor.Conventional recovery method is directly reaction mother liquor to be distilled in reactor, and toluene and water are distilled out of with the form of azeotrope, pass through circulating water condensing, obtain the mixed solution of toluene and water, mixed solution stratification, reclaims upper toluene clear liquid, dry through drying tower, toluene recovery the most at last.Rest materials in reactor, after deionized water wash, is sent into vacuum filtration cylinder and is carried out solid-liquid separation, obtains the intermediates of nucleator, then sends into next procedure and carries out nucleator production.In the production of polypropylene nucleater, according to the difference of nucleator kind, except selecting toluene to do solvent, also can select the multi-solvents such as tetrahydrofuran (THF), hexanaphthene, methyl alcohol, halohydrocarbon, but substantially take the method for directly distilling for the recovery of solvent in reactor, described in patent CN 101367833A, CN 1803900A, after reaction finishes, directly in reactor, distill with desolvation.
The subject matter that conventional method for recovering solvents exists is that thermo-efficiency is low, energy consumption is high, because the method for straight run distillation normally heats by the chuck of reactor, heat transfer efficiency is lower; And, for adopting the nucleator production process that toluene is solvent, in reaction mother liquor, except containing solvent toluene, also have the intermediates of nucleator and a large amount of water, adopt the mode of straight run distillation, steam consumption is larger.
In patent CN 102250398A, mention, after nucleator reaction finishes, adopt the mode of press filtration to reclaim solvent, but for the mother liquor of the polypropylene nucleater described in this patent, its main component is toluene, water, triethylamine salt and a small amount of impurity.Wherein, toluene and water do not dissolve each other, and triethylamine salt and partial impurities are dissolved in water, and all the other impurity are mainly the intermediates of nucleator, are suspended state in water, therefore adopt the mode of press filtration, cannot reclaim and obtain pure solvent.
Summary of the invention
In order to solve above-mentioned technical problem of the prior art, the invention provides a kind of method that reclaims toluene from the mother liquor of production polypropylene nucleater.First reaction product is carried out to solid-liquid separation, then carry out oily water separation to separating mother liquor, finally distill oil phase and reclaim toluene.The method has obviously improved Energy efficiency, and not only toluene quality and the rate of recovery are higher, and has reduced steam consumption, reaches the object of energy-conserving and environment-protective.
" recovery method of toluene in a kind of solvent of producing polypropylene nucleater " of the present invention is achieved in that
A method that reclaims toluene from the mother liquor of production polypropylene nucleater, the method comprises the following steps successively:
(1) solid-liquid separation: after polypropylene nucleater reaction finishes, first, by reaction product stratification in reactor, the mother liquor then layering being obtained is delivered in retort;
(2) oily water separation: contain toluene and water in described mother liquor, first carry out stratification at described retort, then retain the upper oil phase that contains toluene that layering obtains, lower floor's water is discharged to described retort;
(3) toluene distillation: at described retort, described oil phase is distilled, the toluene that after distillation, condensation is got off enters lime set tank;
(4) toluene is dry: after being dried from the toluene of described lime set tank, enter toluene tank.
In the specific implementation, contain the intermediates of toluene, water, triethylamine salt and nucleator in described mother liquor, the intermediates of described nucleator are suspended state in water.
In the specific implementation, in step (1), be provided with suction filtration head in described reactor, 600 ~ 1000 object screen clothes are installed in described suction filtration head, the mother liquor that described layering obtains is pumped to retort by described suction filtration head vacuum.Rest materials in described reactor, carries out centrifugation, and separating obtained filtrate enters in described retort, and separating obtained filter cake returns in described reactor, adds deionized water to open agitator treating filter cake, and washing water enter in described retort.The operation of above-mentioned centrifugation, deionized water wash is carried out 2 ~ 4 times altogether, and wherein the washing water of 1 ~ 2 operation enter in described retort, after washing water be several times collected in washing water pot.
In step (2), described retort is sloping bottom tank, and its cone angle is 40 ~ 60 °, and described retort is provided with interior heating coil, passes into heating agent and carry out toluene distillation in coil pipe.In step (3), in described lime set tank, be provided with interior spiral coil cooling tube, to prevent toluene volatilization.In step (4), toluene is removed moisture in drying tower.
The method that reclaims toluene from the mother liquor of production polypropylene nucleater provided by the invention, first reaction mother liquor is carried out to solid-liquid separation, again by liquid phase stratification, discharge lower floor's water, under the condition of normal pressure or decompression, upper oil phase is distilled, then through condensation, dry, the toluene after being purified, the present invention has greatly reduced steam consumption, thereby reaches the object of energy-conserving and environment-protective.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of toluene recovery method of the present invention.
Nomenclature:
1. reactor 2. separating centrifuge 3. retort 4. condenser 5. lime set tank 6. toluene pump 7. drying tower 8. treatment tank 9. pumped vacuum systems 10. are washed water pot 11. water pumps 12. and are looked cup
Embodiment
Be described in further detail technical scheme of the present invention below in conjunction with drawings and Examples, protection scope of the present invention is not limited to following embodiment.
Embodiment 1
After the nucleator reaction in reactor 1 finishes, the material composition in reactor 1 and content are in table 1.Toluene recovery is operating as periodical operation, the present invention to the calculating of each material mass and energy consumption take batch as calculate basis.
Table 1
(1) solid-liquid separation
After nucleator reaction in reactor 1 finishes, static 30min, is designed with suction filtration head in reactor 1, and suction filtration head is connected with retort 3 by pipeline, 800 object screen clothes is installed, to prevent that solid materials from entering in suction filtration head.
Start pumped vacuum systems 9, make the certain vacuum tightness of the interior maintenance of retort 3, the liquid phase of the reactor 1 interior overwhelming majority is by suction filtration head, be extracted in retort 3, then close pumped vacuum systems 9, open two valves of reactor 1 below, make in reactor 1 gravity flow of remaining material enter separating centrifuge 2 and carry out centrifugation.The main component of isolating filtrate is toluene, water, triethylamine salt and a small amount of impurity, and the main component of filter cake is the intermediates of nucleator.
For preventing the material such as residual toluene in filter cake, need wash filter cake.Deionized water in washing water pot 10 is delivered in reactor 1 through water pump 11, and filter cake manually joins in still by the solid feed inlet of reactor, opens and stirs, and washs.After washing finishes, repeat the operations such as suction filtration, centrifugation.
To filtrate sampling analysis, guarantee that the pH value of filtrate is between 6 ~ 7, otherwise, need again wash.1st, the gravity flow of 2 centrifugations obtain filtrate enters retort 3, after the filtrate gravity flow that obtains of centrifugation several times enter washing water pot 10, use as next round washing leaching cake.
(2) profit layering
(3) toluene distillation
Approximately 111 ℃ of the boiling point of toluene under normal pressure, are provided with interior heating coil in retort 3, tank dresses outside heat-insulating heat-preserving material.Adopt the heating agent of 0.3MPa steam as retort 3.The toluene vapor steaming enters the shell side condensation of condenser 4, and the tube side of condenser passes into water at low temperature (refrigerant), and upper water temp is 10 ℃, and return water temperature is 15 ℃, and toluene is condensed to 25 ℃, and the gravity flow of toluene phlegma enters in lime set tank 5.For reducing the volatilization of toluene, in lime set tank 5, be provided with interior spiral coil cooling tube, in pipe, pass into water at low temperature cooling, lime set tank 5 dresses outside cold insulation material.
(4) dry
After toluene distillation finishes, the toluene in lime set tank 5 is delivered to drying tower 7 by toluene pump 6 and is dried, the interior filling of drying tower 7
molecular sieve, toluene enters from the bottom of drying tower 7, flows out from the top of drying tower 7, enters in treatment tank 8 through the toluene gravity flow of super-dry, and for subsequent use, the interior filling for the treatment of tank 8 is a certain amount of
molecular sieve.
Calculate the energy consumption of toluene air distillation process, and amount to into standard oil, the results are shown in Table 2.
Table 2
Consider the low-grade heat source that makes full use of factory, as steam condensate, can make above-mentioned toluene air distillation into underpressure distillation, working pressure scope-101.3kPa～0(gauge pressure).And, adopting the thermal source of steam condensate as retort 3, the vacuum tightness in retort 3 realizes by pumped vacuum systems 9.In toluene distillation process, lime set tank 5 is connected by pipeline with pumped vacuum systems 9, thereby guarantees to exist in system certain vacuum tightness.
Comparative example 1
Adopt traditional technology to reclaim the toluene in mother liquor.Removal process comprises:
(1) toluene distillation
After the nucleator reaction in reactor finishes, continue to pass into steam in the chuck of reactor, reaction mother liquor is distilled, toluene and water are distilled out of with the form of azeotrope, and azeotropic consists of toluene 81.4wt%, water 18.6wt%, working pressure is normal pressure, and service temperature is 84 ℃.After distillation finishes, the intermediates of remaining nucleator, need wash by deionized water, to remove residual impurity.
(2) condensation
The toluene distilling out and the steam of water, after condenser condenses, are collected in tank.In traditional solvent recovery process, conventionally adopt the steam of circulating water condensing toluene and water, in this comparative example, for convenience of carrying out energy consumption comparison with this patent, design adopts water at low temperature to carry out condensation to the steam of toluene and water.The upper water temp of water at low temperature is 10 ℃, and return water temperature is 15 ℃, and the mixture of toluene and water is condensed to 25 ℃.
(3) profit layering
To be collected in the mixture stratification 2 hours of toluene in tank and water, after layering, upper strata is toluene phase, and lower floor is water, and water is given off to system, collects toluene phase.
(4) dry
Toluene is delivered to drying tower and be dried, to remove the micro-moisture containing in toluene.
Calculate the energy consumption of toluene recovery process in traditional technology, and amount to into standard oil, the results are shown in Table 3.
Table 3
Can find by contrast, in the present invention, adopt the method for pre-separation, greatly reduce the consumption of steam, although because the use of separating centrifuge has increased power consumption, but from whole system, not only toluene guarantees that yield is high, good product quality, and has obvious energy-saving effect.
Claims (8)
1. a method that reclaims toluene from the mother liquor of production polypropylene nucleater, the method comprises the following steps successively:
(1) solid-liquid separation: after polypropylene nucleater reaction finishes, first, by reaction product stratification in reactor, the mother liquor then layering being obtained is delivered in retort;
(2) oily water separation: contain toluene and water in described mother liquor, first carry out stratification at described retort, then retain the upper oil phase that contains toluene that layering obtains, lower floor's water is discharged to described retort;
(3) toluene distillation: at described retort, described oil phase is distilled, the toluene that after distillation, condensation is got off enters lime set tank;
(4) toluene is dry: after being dried from the toluene of described lime set tank, enter toluene tank.
2. recovery method according to claim 1, is characterized in that:
In step (1), in described reactor, be provided with suction filtration head, 600 ~ 1000 object screen clothes are installed in described suction filtration head, the mother liquor that described layering obtains is pumped to retort by described suction filtration head vacuum.
3. recovery method according to claim 2, is characterized in that:
In step (1), the rest materials in described reactor, carries out centrifugation, and separating obtained filtrate enters in described retort, and separating obtained filter cake is with deionized water wash in described reactor, and washing water enter in described retort.
4. recovery method according to claim 3, is characterized in that:
Rest materials in described reactor, carries out the operation of 2 ~ 4 described centrifugations, deionized water wash, and wherein the washing water of 1st ~ 2 operations enter in described retort.
5. recovery method according to claim 1, is characterized in that:
In step (2), described retort is sloping bottom tank, and its cone angle is 40 ~ 60 °, and described retort is provided with interior heating coil.
6. recovery method according to claim 1, is characterized in that:
In step (3), in described lime set tank, be provided with interior spiral coil cooling tube.
7. recovery method according to claim 1, is characterized in that:
In step (4), toluene is removed moisture in drying tower.
8. recovery method according to claim 1, is characterized in that:
In described mother liquor, contain the intermediates of toluene, water, triethylamine salt and nucleator, the intermediates of described nucleator are suspended state in water.
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| CN201210429978.0A CN103787820B (en) | 2012-10-31 | 2012-10-31 | A kind of method reclaiming toluene from the mother liquor producing polypropylene nucleater |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949024A (en) * | 2016-05-14 | 2016-09-21 | 宁波市天普橡胶科技有限公司 | Methylbenzene recycling device of rubber pipe extruding production line |
| CN111111248A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | Device and method for recovering toluene from organic solvent for preparing polyolefin catalyst |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3466345A (en) * | 1967-05-29 | 1969-09-09 | Universal Oil Prod Co | Aromatic hydrocarbon recovery process |
| CN1047668A (en) * | 1989-06-02 | 1990-12-12 | 岳阳石油化工总厂研究院 | A kind of method that reclaims epoxy chloropropane and toluene |
| CN101624327A (en) * | 2009-08-14 | 2010-01-13 | 山西恒扬科技有限公司 | Method for preparing methylbenzene or dimethylbenzene by alkylating benzene with methanol |
-
2012
- 2012-10-31 CN CN201210429978.0A patent/CN103787820B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3466345A (en) * | 1967-05-29 | 1969-09-09 | Universal Oil Prod Co | Aromatic hydrocarbon recovery process |
| CN1047668A (en) * | 1989-06-02 | 1990-12-12 | 岳阳石油化工总厂研究院 | A kind of method that reclaims epoxy chloropropane and toluene |
| CN101624327A (en) * | 2009-08-14 | 2010-01-13 | 山西恒扬科技有限公司 | Method for preparing methylbenzene or dimethylbenzene by alkylating benzene with methanol |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105949024A (en) * | 2016-05-14 | 2016-09-21 | 宁波市天普橡胶科技有限公司 | Methylbenzene recycling device of rubber pipe extruding production line |
| CN105949024B (en) * | 2016-05-14 | 2019-02-22 | 宁波市天普橡胶科技有限公司 | A kind of toluene recovery device of rubber tube extruding production line |
| CN111111248A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | Device and method for recovering toluene from organic solvent for preparing polyolefin catalyst |
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