CN102079687B - Recycling method of residual liquor in production of trichloroethylene - Google Patents
Recycling method of residual liquor in production of trichloroethylene Download PDFInfo
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- CN102079687B CN102079687B CN 201010593059 CN201010593059A CN102079687B CN 102079687 B CN102079687 B CN 102079687B CN 201010593059 CN201010593059 CN 201010593059 CN 201010593059 A CN201010593059 A CN 201010593059A CN 102079687 B CN102079687 B CN 102079687B
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Abstract
The invention relates to a recycling method of residual liquor in the production of trichloroethylene. The method comprises the following steps: residual liquor is collected in a top solution container and enters an alkaline washing tower to neutralize the acid in the residual liquor; the pretreated residual solution enters a distillation kettle to perform distillation, wherein the temperature of the distillation kettle is kept to 85-95 DEG C and dichloroethylene, trichloroethylene and tetrachloroethylene are distilled; the distilled dichloroethylene, trichloroethylene and tetrachloroethylene enter a rectifying tower to perform atmospheric distillation, wherein dichloroethylene is distilled at 42+/-1 DEG C, trichloroethylene is distilled at 87+/-1 DEG C and tetrachloroethylene is distilled at 121+/-1 DEG C; when the pressure of the distillation kettle is vacuumized to -80kPa, tetrachloroethylene is separated at 90+/-1 DEG C and pentachloroethane is obtained in the distillation kettle. According to the method in the invention, all the components of the residual liquor can be completely separated, the zero emission of residues can be realized, the whole production process can realize closed circulation, the pollutions to the environment can be reduced, the residual liquor can be fully utilized, the recycling rate is high and the product yield can be increased.
Description
Technical field
The present invention relates to the recovery method of raffinate in a kind of trieline production, belong to chemical technology field.
Background technology
In the production process of trieline, the residue of generation, raffinate amount are very large, and the volume ratio of each main component in residue, the raffinate is: tetrachloroethane 30%; Trieline 30%; Zellon 10%; Pentaline 10%; Trichloroethane 10%; Other 10%, each comparison of ingredients complexity and boiling point are more close in the raffinate, are difficult to separate fully by rectification process.Common treating method is that these residues, raffinate are directly entered in the environment, understands like this serious environment pollution, can bring very large potential safety hazard simultaneously.Environmental pollution is serious, and be affects the principal element that trieline is produced always.
At present, trieline manufacturing enterprise is to residue, raffinate Adopts measure: measure more several sorbent materials to the regeneration effect of trieline absorption and different regenerations, adopt the alternating temperature pressure-variable adsorption, utilize purified gas thermal regeneration sorbent material to remove and to reclaim the technique of trieline, adopt above technique to reclaim residue, raffinate, construction equipment is huge, complex process, need to consume a large amount of energy, seriously polluted, cost recovery is high, and the rate of recovery is low.
Be 931115957 such as application number, open day is the Chinese patent on September 14th, 1994, discloses a kind of method for refining of trieline, through rectifying purification, filtering and impurity removing, installed to the technological process of finished product in clean minute; Before rectifying purifies first through primary purification and the drying two road techniques that dewater; Primary purification adds the distilled water that contains silver ammino solution of 1.5 times of trieline weight for the technical grade trieline is put into reactor, carries out mechanical stirring 2 hours, and layering in rear static 30 minutes sucks upper water; Drying dewaters as in the trieline behind primary purification, and adding is the discolour silica gel of trieline 1/10 left and right sides volume ratio, and shake well makes trace water by silica gel adsorption, trieline is taken out in static filtration, and defective is that generation waste water is more, trieline after the recovery is second-rate, and purity is low.
Summary of the invention
The technical problem to be solved in the present invention is for above deficiency, the recovery method of raffinate in a kind of trieline production is provided, adopts the method that raffinate is reclaimed, recovery utilization rate is high, realize the zero release of raffinate in the trieline production, reduced pollution and production cost to environment.
For overcoming the above problems, technical scheme of the present invention is as follows: the recovery method of raffinate during a kind of trieline is produced, and it is characterized in that: described recovery method may further comprise the steps:
A, pre-treatment: the raffinate that produces in the trieline production process is collected in the flow container of top, enter again in the soda-wash tower in and the acid in the raffinate;
B, distillation: pretreated raffinate enters in the still kettle and distills, and the temperature of still kettle remains between 85 ℃-95 ℃, distills out Ethylene Dichloride, trieline and zellon;
C, rectifying: the Ethylene Dichloride that distills out, trieline and zellon enter and carry out atmospheric distillation in the rectifying tower, distill out Ethylene Dichloride in the time of 42 ± 1 ℃, distill out trieline in the time of 87 ± 1 ℃, distill out zellon in the time of 121 ± 1 ℃;
After d, zellon rectifying are finished, with being evacuated to 80 kPas of negative pressure in the still kettle, in the time of 90 ± 1 ℃, isolate tetrachloroethane;
E, distill out tetrachloroethane after, in still kettle, obtain pentaline.
As further improvement in the technical proposal:
Among the step a, it is 0.5% NaOH solution that soda-wash tower contains concentration.
Among the step b, pretreated raffinate collects in first in the flow container of neutralization top, then enters still kettle from neutralization top flow container.
Among the step c, the Ethylene Dichloride that distills out enters in the return tank after entirely coagulating gas condenser and the condensation of TCE tail cooler through TCE, enters in the azeotrope tank again, then enters in the still kettle.
Among the step c, the trieline that distills out enters in the return tank after entirely coagulating gas condenser and the condensation of TCE tail cooler through TCE, then enters the middle runnings tank.
Among the step c, the zellon that distills out enters in the return tank after entirely coagulating gas condenser and the condensation of TCE tail cooler through TCE, then enters in the after cut tank.
In the steps d, with pressure pump and squirt pump still kettle is vacuumized negative-pressure operation, isolated tetrachloroethane enters in the return tank after still kettle process complete condenser, the condensation of tail cooler, be pooled to the tetrachloroethane tank stores, enter again in the still kettle again rectification and purification.
When the still kettle liquid level descends 1/5 the time, close squirt pump, in soda-wash tower, add raffinate.
The present invention adopts above technical scheme, compared with prior art, has the following advantages:
(1) utilizes this recovery method, the various compositions in the raffinate all can be separated, realized the zero release of residue, make whole production technique reach sealing and circulating, reduced the pollution to environment.
(2) raffinate in the trieline production is fully used, and recovery utilization rate is high, has improved product yield, has saved production cost, has improved economic benefit.
The present invention will be further described below in conjunction with drawings and Examples.
Description of drawings
Accompanying drawing is to reclaim process flow sheet in the embodiment of the invention.
Among the figure,
1-top flow container, 2-charge pump, 3-alkali liquid tank, 4-lye pump, the 5-still kettle, 6-take away pump, 7-tetrachloroethane tank, 8-tail tank, the 9-pressure pump, the 10-soda-wash tower, among the 11-and the flow container of top, the 12-rectifying tower, 13-TCE is solidifying gas condenser entirely, 14-azeotrope tank, 15-return tank, 16-middle runnings tank, 17-TCE tail cooler, 18-after cut tank, 19-complete condenser, 20-gas-liquid separator, 21-tail cooler, 22-surge tank, 23-squirt pump.
Specific embodiment
Embodiment, the recovery method of raffinate during a kind of trieline is produced may further comprise the steps:
The raffinate that produces in the trieline production process is collected in the top flow container 1, pump in the soda-wash tower 10 with charge pump 2,0.5% NaOH solution is arranged in the soda-wash tower 10, be used for and raffinate in acid, after soda-wash tower 10 pre-treatment, raffinate collects in the neutralization top flow container 11, neutralization top flow container 11 interior Ethylene Dichloride content about 5%, trieline content about 65%, zellon content about 20%, tetrachloroethane content about 5%, pentaline content about 5%, then Ethylene Dichloride, trieline, zellon, tetrachloroethane and pentaline enter still kettle 5 and distill, each component is separated in the still kettle 5 interior differences of boiling point of utilizing, still kettle 5 is used steam heating, temperature remains between 85 ℃-95 ℃, distill out Ethylene Dichloride, trieline and zellon, Ethylene Dichloride, trieline and zellon enter and carry out rectifying in the rectifying tower 12, Ethylene Dichloride, trieline and zellon carry out the cut in early stage in the rectifying tower 12 interior differences of boiling point of utilizing, middle runnings separates with the later stage cut, adopt atmospheric operation, early stage, cut was Ethylene Dichloride, in the time of 42 ± 1 ℃, steam Ethylene Dichloride, Ethylene Dichloride enters in the return tank 15 after entirely coagulating gas condenser 13 and 17 condensations of TCE tail cooler through TCE, purity is more than 90%, enter again in the azeotrope tank 14, and then enter in the still kettle 5; Middle runnings is trieline, steams trieline at 87 ± 1 ℃, and process TCE enters in the return tank 15 after entirely coagulating gas condenser 13 and 17 condensations of TCE tail cooler, and then purity enter middle runnings tank 16 from return tank 15 more than 99.9%; The later stage cut is zellon, steams zellon at 121 ± 1 ℃, and process TCE enters in the return tank 15 after entirely coagulating gas condenser 13 and 17 condensations of TCE tail cooler, and then purity enter the after cut tank 18 from return tank 15 more than 90%;
When 121 ± 1 ℃ of temperature departures, zellon rectifying is finished, high boiling material tetrachloroethane in the raffinate and pentaline can't continue to distill out, need to open 23 pairs of still kettles 5 of pressure pump 9 and squirt pump this moment and vacuumize negative-pressure operation to separate the higher tetrachloroethane of boiling point, utilize 80 kPas of negative pressure, in the time of 90 ± 1 ℃, separate tetrachloroethane, tetrachloroethane is from still kettle 5 process complete condensers 19, after 21 condensations of tail cooler, enter in the return tank 20, purity is pooled at last tetrachloroethane tank 7 and stores, after tank is full more than 95%, be transmitted back to take away pump 6 and again participate in rectifying in the still kettle 5, further purifying reaches 99.99%.
When still kettle 5 liquid levels descend 1/5 the time, close squirt pump 23, start charge pump 2 to soda-wash tower 10 next batch of material of interior adding.Repeat aforesaid operations, until raffinate is disposed.The material water white transparency that steams enters next treatment system, still kettle 5 interior remainders be pentaline, purity is more than 85%, can be used as high boiling material and sells.
Top flow container 1, alkali liquid tank 3, tetrachloroethane tank 7, neutralization top flow container 11, azeotrope tank 14, return tank 15, middle runnings 16, after cut tank 18 and surge tank 22 are chemical industry hold-up vessel commonly used,
TCE entirely solidifying gas condenser 13, TCE tail cooler 17, complete condenser 19 and tail cooler 21 is chemical industry condenser commonly used.
Above equipment is chemical industry equipment commonly used.
Claims (1)
1. the recovery method of raffinate during a trieline is produced, it is characterized in that: described recovery method may further comprise the steps:
A, pre-treatment: the raffinate that produces in the trieline production process is collected in the top flow container (1), enter again in the soda-wash tower (10) in and the acid in the raffinate;
B, distillation: pretreated raffinate enters in the still kettle (5) and distills, and the temperature of still kettle (5) remains between 85 ℃-95 ℃, distills out Ethylene Dichloride, trieline and zellon;
C, rectifying: the Ethylene Dichloride that distills out, trieline and zellon enter in the rectifying tower (12) and carry out atmospheric distillation, distill out Ethylene Dichloride in the time of 42 ± 1 ℃, distill out trieline in the time of 87 ± 1 ℃, distill out zellon in the time of 121 ± 1 ℃;
After d, zellon rectifying are finished, with being evacuated to 80 kPas of negative pressure in the still kettle (5), in the time of 90 ± 1 ℃, isolate tetrachloroethane;
E, distill out tetrachloroethane after, in still kettle (5), obtain pentaline;
Among the step a, it is 0.5% NaOH solution that soda-wash tower (10) contains concentration;
Among the step b, pretreated raffinate collects in first in the neutralization top flow container (11), then enters still kettle (5) from neutralization top flow container (11);
Among the step c, the Ethylene Dichloride that distills out enters in the return tank (15) after entirely coagulating gas condenser (13) and TCE tail cooler (17) condensation through TCE, enters in the azeotrope tank (14) again, then enters in the still kettle (5);
Among the step c, the trieline that distills out enters in the return tank (15) after entirely coagulating gas condenser (13) and TCE tail cooler (17) condensation through TCE, then enters middle runnings tank (16);
Among the step c, the zellon that distills out enters in the return tank (15) after entirely coagulating gas condenser (13) and TCE tail cooler (17) condensation through TCE, then enters in the after cut tank (18);
In the steps d, with pressure pump (9) and squirt pump (23) still kettle (5) is vacuumized negative-pressure operation, isolated tetrachloroethane is after still kettle (5) process complete condenser (19), tail cooler (21) condensation, enter in the return tank (20), be pooled to tetrachloroethane tank (7) and store, enter again in the still kettle (5) again rectification and purification;
When still kettle (5) liquid level descends 1/5 the time, close squirt pump (23), in soda-wash tower (10), add raffinate.
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| CN 201010593059 CN102079687B (en) | 2010-12-17 | 2010-12-17 | Recycling method of residual liquor in production of trichloroethylene |
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| CN104045468A (en) * | 2014-07-05 | 2014-09-17 | 山东史贝美肥料股份有限公司 | Special functional urea formaldehyde fertilizer for garlic and preparation method thereof |
| CN105859511B (en) * | 2016-05-24 | 2019-01-04 | 芜湖融汇化工有限公司 | The separator and separation method of TCE by-product low-boiling-point substance |
| CN106946649A (en) * | 2017-02-24 | 2017-07-14 | 芜湖融汇化工有限公司 | Material deacidification device in trichloro ethylene system |
| CN117843441A (en) * | 2024-03-07 | 2024-04-09 | 山东新龙科技股份有限公司 | High-boiling-point substance treatment method and device in trichloroethylene production |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092057A (en) * | 1993-07-27 | 1994-09-14 | 江阴市化工试剂研究所 | The method for refining of trieline |
| CN101353289A (en) * | 2008-08-19 | 2009-01-28 | 何勇志 | Method for extracting trans-dichloroethylene from low-boiling residue of ethinyltrichloride production by gas-phase catalytic process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7268262B2 (en) * | 2004-04-29 | 2007-09-11 | Ppg Industries Ohio, Inc. | Method for recovering trans-1,2-dichloroethene |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092057A (en) * | 1993-07-27 | 1994-09-14 | 江阴市化工试剂研究所 | The method for refining of trieline |
| CN101353289A (en) * | 2008-08-19 | 2009-01-28 | 何勇志 | Method for extracting trans-dichloroethylene from low-boiling residue of ethinyltrichloride production by gas-phase catalytic process |
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Effective date of registration: 20230620 Address after: 262700 No. 26, Tianliu Section, No.3 Road, Tianliu Town, Shouguang City, Weifang City, Shandong Province Patentee after: SHANDONG XINLONG TECHNOLOGY Co.,Ltd. Address before: 262700 Shandong Province, Shouguang City Tian Ryu Jin Xinlong Industrial Park Patentee before: SHANDONG XINLONG PVC Co.,Ltd. |