CN103382069B - Processing method of waste liquid in glycol recycling device - Google Patents

Processing method of waste liquid in glycol recycling device Download PDF

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Publication number
CN103382069B
CN103382069B CN201310261225.8A CN201310261225A CN103382069B CN 103382069 B CN103382069 B CN 103382069B CN 201310261225 A CN201310261225 A CN 201310261225A CN 103382069 B CN103382069 B CN 103382069B
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heavy alcohol
retort
waste liquid
transporting
receiving tank
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CN103382069A (en
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李来福
李海涛
王斌
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Henghe Materials and Science Technology Co Ltd
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ZHEJIANG HENGHE PETROCHEMICAL CO Ltd
Ningbo Polytechnic
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Abstract

The invention relates to a processing method of waste liquid in a glycol recycling device. The method comprises following steps: (1) transporting the heavy alcohol waste liquid to a heat exchanger through a delivery pump, after the heavy alcohol waste liquid exchanges heat with the high-temperature heavy alcohol gas which is fractionated through a retort, transporting the heavy alcohol waste liquid to a distillation still to subject to a reduced pressure distillation treatment; (2) performing a swift operation of the distillation still, transporting the heavy alcohol separated from the top of the distillation distill to a condenser, collecting the condensed liquid with a collecting tank; (3) transporting the waste salt separated by the distillation still to a retort trough a conveyor belt, transporting the heavy alcohol which overflows out of the conveyor belt to a settling tank, after the materials in the settling tank precipitate, transporting the heavy alcohol in the upper part to a receiving tank, transporting the materials in the bottom to the raw material pool at fixed periods; (4) subjecting the waste salt in the retort to a dry distillation treatment by a hot-air blower, transporting the heavy alcohol gas to a heat exchanger, then condensing the heavy alcohol gas, transporting the condensed heavy alcohol liquid to a receiving tank, and packaging the waste salt in the bottom of the retort. The processing method of waste liquid in a glycol recycling device has the advantages of simple operation and suitability for industrial implementation, and the heavy alcohol and waste salt in the recycle waste liquid can be effectively recycled.

Description

A kind for the treatment of process of glycol recovery device waste liquid
Technical field
The invention belongs to industrial glycol recovery field, particularly a kind for the treatment of process of glycol recovery device waste liquid.
Background technology
At present, when waste liquid carries out glycol recovery distillation in to ethylene oxide production plant, can produce the thickness waste liq that a large amount of heavy alcohol and salts substances mix, this waste liquid has wetting ability, when heat, be dissolved in together, when cold, be just mixed to form colloidalmaterial, difficult treatment.Untreated waste liquid is without any commodity value, and this waste liquid environmental pollution is more serious, affects the production environment of whole glycol recovery device, is the production difficult problem that glycol recovery device exists always.
The domestic upper processing to this waste liquid is mainly following several method: (1), by this waste liquid is carried out to burning disposal, the bits that produce after burning are carrying out landfill; The method fails effectively to utilize the heavy alcohol in waste liquid, and the waste gas producing in burning process is again by contaminate environment.(2) regulate pH value by water flowing in waste liquid, the heavy alcohol in waste liquid is extracted; Although the method reclaims the heavy alcohol in waste liquid, the salts substances in this waste liquid has been dissolved in water, and the liquid waste disposal of generation is still very difficult.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind for the treatment of process of glycol recovery device waste liquid, and the method is simple to operate simple, is applicable to industrial implementation, effectively heavy alcohol and the abraum salt in Recycling of waste liquid.
The treatment process of a kind of glycol recovery device waste liquid of the present invention, comprising:
(1) heavy alcohol waste liquid is transported to heat exchanger through transferpump, is undertaken after heat exchange by 400~450 DEG C heavy alcohol gases that fractionate out with retort, is transported to still kettle and carries out underpressure distillation;
(2) still kettle is carried out blocked operation, and the isolated heavy alcohol in still top is transported to condenser, arrives receiving tank after condenser condenses;
(3) the isolated abraum salt of still kettle, is transported to retort through travelling belt, and travelling belt overflow heavy alcohol is out transported to slurry tank, and after the material precipitation in slurry tank, the heavy alcohol in top is transported to receiving tank, and bottom material regularly returns to feed reservoir;
(4) abraum salt in retort is carried out to destructive distillation processing with calorifier, heavy alcohol gas is transported to receiving tank after over-heat-exchanger and condenser condenses, the abraum salt pack packing of retort bottom.
The still kettle of described step (1) heats by outside chuck.
The distillation temperature of described step (1) is 200~260 DEG C, operating pressure-0.9MPa~-0.05MPa.
Described distillation temperature is 230~260 DEG C, operating pressure-0.1MPa~-0.06MPa.
In described step (3), travelling belt top arranges overflow port, and bottom arranges liquid collection trough; Travelling belt overflow heavy alcohol out flows into receiving tank, then by receiving tank, weight alcohol is discharged to slurry tank.
In described step (4), retort bottom adopts spiral discharging valve.
The present invention recycles the heavy alcohol in waste liquid by still kettle and retort, improve waste liquid value-added content of product, by retort, abraum salt has been carried out to destructive distillation processing, at the bottom of still, adopted the method for spiral blanking, to abraum salt pack packing, solve the problem of this liquid waste disposal difficulty contaminate environment.
The present invention adopts the heat of heat exchanger counterweight alcohol gas to reclaim, and effectively utilizes used heat, has reduced plant energy consumption.
beneficial effect
(1) the present invention is simple to operate, and waste liquid is processed, and cost is low, not high to equipment requirements, is applicable to industrial implementation.
(2) counterweight alcohol of the present invention is recycled, and has improved value-added content of product; The abraum salt producing is carried out to destructive distillation pack and process, solved problem of environmental pollution.
Brief description of the drawings
Fig. 1 is device of the present invention and schema;
E1 is heat exchanger, and E2, E3 are water cooler, and R1, R2 are still kettle (heating of outside chuck), and C1, C2 are travelling belt, and V1 is slurry tank, and V2 is holding tank, and D1 is retort, and K1 is calorifier, and P1, P2, P3 are transferpump.F1~F11 is material related in the present invention;
F1 be waste liquid, the F2 in glycol recovery device be the isolated abraum salt of still kettle, F3 be the isolated heavy alcohol gas of still kettle, F4 be from heavy alcohol lime set, the F5 of still kettle be from heavy alcohol liquid, the F6 of slurry tank be from heavy alcohol gas, the F7 of retort be from heavy alcohol lime set, the F8 of retort be from heavy alcohol liquid, the F9 of Receiving bin attach most importance to that alcohol is sent outside, F10 is abraum salt pack, F11 is high temperature air.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Raw material:
From the waste liquid in glycol recovery device.Its composition is in table 1
Table 1 waste liquid composition
Embodiment 1
Heavy alcohol waste liquid F1 temperature after heat exchanger E1 and heavy alcohol gas F6 carry out heat exchange is 120 DEG C, enter still kettle R1/R2, distillation temperature is 230 DEG C, operating pressure carries out blocked operation, after the liquid level of one of them still reaches 80%, is switched to another for-0.07MPa(two still kettles).From still kettle, heavy alcohol gas F3 is out transported to receiving tank V2 after condenser E2 condensation, at the bottom of still kettle still, material F2 is out sent to retort D1 through travelling belt C1/C2, travelling belt overflow material out flows into slurry tank V1 after receiving tank is collected, the material F8 on slurry tank top is transported to receiving tank V2, enter the abraum salt of retort and carry out heat exchange from the high temperature air of calorifier K1, retort service temperature is 500 DEG C.From retort, heavy alcohol gas F6 out removes receiving tank V2 after heat exchanger and condenser E3 condensation, and retort bottom is through the material F10 pack out of spiral discharging valve.
The heavy alcohol F9 of receiving tank, with its heavy alcohol content of gas chromatographic analysis, water-content, and measures its solid contents, fixed its solids content of retort abraum salt F10 side out, and what obtain the results are shown in Table 2.
Embodiment 2
Waste liquid F1 temperature after heat exchanger E1 and heavy alcohol gas F6 carry out heat exchange is 120 DEG C, enter still kettle R1/R2, distillation temperature is 230 DEG C, and operating pressure carries out blocked operation, after the liquid level of one of them still reaches 80%, is switched to another for-0.08MPa(two still kettles).From still kettle, heavy alcohol gas F3 is out transported to receiving tank V2 after condenser E2 condensation, at the bottom of still kettle still, material F2 is out sent to retort D1 through travelling belt C1/C2, travelling belt overflow material out removes slurry tank V1 after receiving tank is collected, the material F8 on slurry tank top is transported to receiving tank V2, enter the abraum salt of retort and carry out heat exchange from the high temperature air of calorifier K1, retort service temperature is 500 DEG C.From retort, heavy alcohol gas F6 out removes receiving tank V2 after heat exchanger and condenser E3 condensation, and retort bottom is through the material F10 pack out of spiral discharging valve.
The heavy alcohol F9 of receiving tank, with its heavy alcohol content of gas chromatographic analysis, water-content, and measures its solid contents, fixed its solids content of retort abraum salt F10 side out, and what obtain the results are shown in Table 2.
Embodiment 3
Waste liquid F1 temperature after heat exchanger E1 and heavy alcohol gas F6 carry out heat exchange is 120 DEG C, enter still kettle R1/R2, distillation temperature is 230 DEG C, and operating pressure carries out blocked operation, after the liquid level of one of them still reaches 80%, is switched to another for-0.06MPa(two still kettles).From still kettle, heavy alcohol gas F3 is out transported to receiving tank V2 after condenser E2 condensation, at the bottom of still kettle still, material F2 is out sent to retort D1 through travelling belt C1/C2, travelling belt overflow material out removes slurry tank V1 after receiving tank is collected, the material F8 on slurry tank top is transported to receiving tank V2, enter the abraum salt of retort and carry out heat exchange from the high temperature air of calorifier K1, retort service temperature is 500 DEG C.From retort, heavy alcohol gas F6 out removes receiving tank V2 after heat exchanger and condenser E3 condensation, and retort bottom is through the material F10 pack out of spiral discharging valve.
The heavy alcohol F9 of receiving tank, with its heavy alcohol content of gas chromatographic analysis, water-content, and measures its solid contents, fixed its solids content of retort abraum salt F10 side out, and what obtain the results are shown in Table 2.
Embodiment 4
Waste liquid F1 temperature after heat exchanger E1 and heavy alcohol gas F6 carry out heat exchange is 120 DEG C, enter still kettle R1/R2, distillation temperature is 250 DEG C, and operating pressure carries out blocked operation, after the liquid level of one of them still reaches 80%, is switched to another for-0.07MPa(two still kettles).From still kettle, heavy alcohol gas F3 is out transported to receiving tank V2 after condenser E2 condensation, at the bottom of still kettle still, material F2 is out sent to retort D1 through travelling belt C1/C2, travelling belt overflow material out removes slurry tank V1 after receiving tank is collected, the material F8 on slurry tank top is transported to receiving tank V2, enter the abraum salt of retort and carry out heat exchange from the high temperature air of calorifier K1, retort service temperature is 500 DEG C.From retort, heavy alcohol gas F6 out removes receiving tank V2 after heat exchanger and condenser E3 condensation, and retort bottom is through the material F10 pack out of spiral discharging valve.
The heavy alcohol F9 of receiving tank, with its heavy alcohol content of gas chromatographic analysis, water-content, and measures its solid contents, fixed its solids content of retort abraum salt F10 side out, and what obtain the results are shown in Table 2.
Embodiment 5
Waste liquid F1 temperature after heat exchanger E1 and heavy alcohol gas F6 carry out heat exchange is 120 DEG C, enter still kettle R1/R2, distillation temperature is 210 DEG C, and operating pressure carries out blocked operation, after the liquid level of one of them still reaches 80%, is switched to another for-0.07MPa(two still kettles).From still kettle, heavy alcohol gas F3 is out transported to receiving tank V2 after condenser E2 condensation, at the bottom of still kettle still, material F2 is out sent to retort D1 through travelling belt C1/C2, travelling belt overflow material out removes slurry tank V1 after receiving tank is collected, the material F8 on slurry tank top is transported to receiving tank V2, enter the abraum salt of retort and carry out heat exchange from the high temperature air of calorifier K1, retort service temperature is 500 DEG C.From retort, heavy alcohol gas F6 out removes receiving tank V2 after heat exchanger and condenser E3 condensation, and retort bottom is through the material F10 pack out of spiral discharging valve.
The heavy alcohol F9 of receiving tank, with its heavy alcohol content of gas chromatographic analysis, water-content, and measures its solid contents, fixed its solids content of retort abraum salt F10 side out, and what obtain the results are shown in Table 2.
Embodiment 6
Waste liquid F1 temperature after heat exchanger E1 and heavy alcohol gas F6 carry out heat exchange is 120 DEG C, enter still kettle R1/R2, distillation temperature is 230 DEG C, and operating pressure carries out blocked operation, after the liquid level of one of them still reaches 80%, is switched to another for-0.07MPa(two still kettles).From still kettle, heavy alcohol gas F3 is out transported to receiving tank V2 after condenser E2 condensation, at the bottom of still kettle still, material F2 is out sent to retort D1 through travelling belt C1/C2, travelling belt overflow material out removes slurry tank V1 after receiving tank is collected, the material F8 on slurry tank top is transported to receiving tank V2, enter the abraum salt of retort and carry out heat exchange from the high temperature air of calorifier K1, retort service temperature is 530 DEG C.From retort, heavy alcohol gas F6 out removes receiving tank V2 after heat exchanger and condenser E3 condensation, and retort bottom is through the material F10 pack out of spiral discharging valve.
The heavy alcohol F9 of receiving tank, with its heavy alcohol content of gas chromatographic analysis, water-content, and measures its solid contents, fixed its solids content of retort abraum salt F10 side out, and what obtain the results are shown in Table 2.
Embodiment 7
Waste liquid F1 temperature after heat exchanger E1 and heavy alcohol gas F6 carry out heat exchange is 120 DEG C, enter still kettle R1/R2, distillation temperature is 230 DEG C, and operating pressure carries out blocked operation, after the liquid level of one of them still reaches 80%, is switched to another for-0.07MPa(two still kettles).From still kettle, heavy alcohol gas F3 is out transported to receiving tank V2 after condenser E2 condensation, at the bottom of still kettle still, material F2 is out sent to retort D1 through travelling belt C1/C2, travelling belt overflow material out removes slurry tank V1 after receiving tank is collected, the material F8 on slurry tank top is transported to receiving tank V2, enter the abraum salt of retort and carry out heat exchange from the high temperature air of calorifier K1, retort service temperature is 480 DEG C.From retort, heavy alcohol gas F6 out removes receiving tank V2 after heat exchanger and condenser E3 condensation, and retort bottom is through the material F10 pack out of spiral discharging valve.
The heavy alcohol F9 of receiving tank, with its heavy alcohol content of gas chromatographic analysis, water-content, and measures its solid contents, fixed its solids content of retort abraum salt F10 side out, and what obtain the results are shown in Table 2.
The each embodiment result of table 2
Title The heavy alcohol content of F9 (%) F9 water-content (%) F9 solid content (%) F10 solid content (%)
Embodiment 1 96.77 3.11 0.12 96.43
Embodiment 2 96.89 3.01 0.1 96.41
Embodiment 3 96.5 3.35 0.15 96.52
Embodiment 4 96.63 3.18 0.19 96.27
Embodiment 5 96.74 3.13 0.13 96.29
Embodiment 6 96.59 3.2 0.21 98.23
Embodiment 7 96.69 3.16 0.15 95.59

Claims (5)

1. a treatment process for glycol recovery device waste liquid, comprising:
(1) heavy alcohol waste liquid is transported to heat exchanger through transferpump, is undertaken after heat exchange by 400~450 DEG C heavy alcohol gases that fractionate out with retort, is transported to still kettle and carries out underpressure distillation;
(2) still kettle is carried out blocked operation, and the isolated heavy alcohol in still top is transported to condenser, arrives receiving tank after condenser condenses;
(3) the isolated abraum salt of still kettle, is transported to retort through travelling belt, and travelling belt overflow heavy alcohol is out transported to slurry tank, and after the material precipitation in slurry tank, the heavy alcohol in top is transported to receiving tank, and bottom material regularly returns to feed reservoir; Wherein, travelling belt top arranges overflow port, and bottom arranges liquid collection trough; Travelling belt overflow heavy alcohol out flows into receiving tank, then by receiving tank, weight alcohol is discharged to slurry tank;
(4) abraum salt in retort is carried out to destructive distillation processing with calorifier, heavy alcohol gas is transported to receiving tank after over-heat-exchanger and condenser condenses, the abraum salt pack packing of retort bottom.
2. the treatment process of a kind of glycol recovery device waste liquid according to claim 1, is characterized in that: the still kettle of described step (1) heats by outside chuck.
3. the treatment process of a kind of glycol recovery device waste liquid according to claim 1, is characterized in that: the distillation temperature of described step (1) is 200~260 DEG C, operating pressure-0.9MPa~-0.05MPa.
4. the treatment process of a kind of glycol recovery device waste liquid according to claim 3, is characterized in that: described distillation temperature is 230~260 DEG C, operating pressure-0.1MPa~-0.06MPa.
5. the treatment process of a kind of glycol recovery device waste liquid according to claim 1, is characterized in that: in described step (4), retort bottom adopts spiral discharging valve.
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CN110128243A (en) * 2019-06-05 2019-08-16 恒河材料科技股份有限公司 A method of propylene glycol in weight alcohol waste liquid is recycled using extraction
CN113717795B (en) * 2021-09-27 2023-11-28 南京林业大学 Novel multifunctional steam distillation-dry distillation integrated equipment

Citations (4)

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Publication number Priority date Publication date Assignee Title
US6048441A (en) * 1997-08-05 2000-04-11 Basf Aktiengesellschaft Isolation of neopentyl glycol hydroxypivalate (NGH)
CN201216885Y (en) * 2008-07-08 2009-04-08 江苏卡特石油新能源有限公司 Methanol recycling apparatus
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CN202440446U (en) * 2012-01-19 2012-09-19 青州天安化工有限公司 Recovery device for methanol

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Publication number Priority date Publication date Assignee Title
US6048441A (en) * 1997-08-05 2000-04-11 Basf Aktiengesellschaft Isolation of neopentyl glycol hydroxypivalate (NGH)
CN201216885Y (en) * 2008-07-08 2009-04-08 江苏卡特石油新能源有限公司 Methanol recycling apparatus
CN101792227A (en) * 2010-03-30 2010-08-04 兖矿鲁南化肥厂 Process equipment containing polyethyleneglycol dimethyl ether and method
CN202440446U (en) * 2012-01-19 2012-09-19 青州天安化工有限公司 Recovery device for methanol

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Address after: 315800 Ningbo, Zhejiang Province, new road, Beilun District No. 1069

Patentee after: Ningbo Polytechnic College

Patentee after: HENGHE MATERIALS & SCIENCE TECHNOLOGY CO., LTD.

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