CN103803691B - A kind of lower concentration formic acid wastewater treatment process - Google Patents
A kind of lower concentration formic acid wastewater treatment process Download PDFInfo
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- CN103803691B CN103803691B CN201410102355.1A CN201410102355A CN103803691B CN 103803691 B CN103803691 B CN 103803691B CN 201410102355 A CN201410102355 A CN 201410102355A CN 103803691 B CN103803691 B CN 103803691B
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Abstract
A kind of lower concentration formic acid wastewater New Process for Treatment, it sprays in esterification-extraction tower by massfraction after the lower concentration formic acid wastewater atomizing spray of 0.1% ~ 3%, and specific liquid rate is 8 ~ 50m
3/ (m
2h), water droplets is uniformly distributed under gravity in tower internal upper part filler, finally natural subsidence in higher alcohols oil phase, 120s is not less than duration of contact with alcohol in settling process, formic acid in water is heated rear and alcohol generation esterification, extract after being converted into corresponding manthanoate in oil phase, temperature of reaction is at 85 ~ 105 DEG C, and temperature of reaction is maintained by the water vapour passed into.Water except formic acid removal continues to fall to tower bottom aquifer, utilizes the initial formic acid wastewater of its heat preheating, for simple biochemical treatment after water layer extraction.By the organic layer extraction of esterification extraction tower bottom to rectifying tower rectification under vacuum, wherein will be separated with alcohol by ester, the highly purified ester of overhead extraction, and send into esterification-extraction tower internal recycle after the high temperature alcohol at the bottom of tower supplements part alcohol and utilize.
Description
Technical field
The present invention relates to a kind for the treatment of process of lower concentration formic acid wastewater.
Background technology
Formic acid (CH
2o
2) also known as making formic acid, colourless and have pungent odour, and be corrosive, boiling point 100.8 DEG C.Because the structure of formic acid is special, its hydrogen atom is directly connected with carboxyl, also can regard a hydroxy carbaldehyde as, and therefore formic acid has the character of acid and aldehyde simultaneously.In chemical industry, formic acid is widely used in the productions such as fabrics printing and dyeing, leather processing, Rubber processing, silage and medicine.
The boiling point of formic acid is 100.8 DEG C, almost with aqueous phase with and dissolve each other with water, Interpolymer Association is extremely strong, if formic acid dilute solution uses distillation method concentrate, poor effect merely.And when temperature is higher, formic acid is volatile.
Table 1: the relation between Analysis of Formic acid Residual and formic acid wastewater temperature
| Temperature/DEG C | 70 | 65 | 60 | 55 | 50 | 45 | 40 | 35 | 30 | 20 |
| Analysis of Formic acid Residual/% | 3.9 | 5.1 | 5.9 | 6.8 | 8.2 | 9.0 | 9.2 | 9.2 | 9.2 | 9.6 |
As shown in table 1, when less than 40 DEG C, the formic acid concn in water is basically stable at about 9.2%, but formic acid concn can sharply decline when the temperature increases, during to 70 DEG C, only has about 4%.Current esterification process process formic acid wastewater, temperature is generally more than 85 DEG C, so be convenient to process when formic acid concn is more than 3% in trade effluent, and when formic acid concn is higher, general usual way is more difficult or processing cost is larger.
At present, the treatment process of being decomposed by formic acid is adopted for containing the research of formic acid treatment of Organic Wastewater, as oxidation style, catalytic decomposition, biochemical treatment process, absorption method and electrolytic process etc., although these method treatment effects are relatively good, but often cost is higher, treatment capacity is very little, is not suitable for industrial applications.Industrial more use rectification method or esterification distillation method or azeotropic-fractionation combine recovery, process formic acid wastewater.Wherein rectification method due to formic acid and water boiling point closely, therefore can not be used alone.The ultimate principle of esterification process makes formic acid and alcohols generation esterification, and reaction equation is as follows:
HCOOH+ROH→HCOOR+H
2O
These class methods adopt esterification usually, rectifying two step completes process to formic acid wastewater, can the higher formic acid wastewater of concentration for the treatment of.For the formic acid wastewater of lower concentration (<4%), water proportion is very high, and when heated waste water and rectifying, required energy consumption is comparatively large, and the cost of process waste water is very high, and formic acid wastewater has corrodibility, can strengthen corrosion sewage treatment equipment under high temperature.
Summary of the invention
The object of this invention is to provide a kind of novel process of lower concentration formic acid wastewater process of less energy-consumption, first in esterification-extraction tower, make formic acid and higher alcohols generation esterification in waste water become ester class, dissolution extraction is in higher alcohols, thus be separated with water, discharge of wastewater after layering, the further rectifying separation ester of oil phase and alcohol, alcohol is reused for esterification-extraction process.
For realizing above-mentioned target, technical scheme of the present invention is as follows:
A kind for the treatment of process of lower concentration formic acid wastewater.Its flow process as shown in Figure 1, comprises the following steps:
(1) will be that the lower concentration formic acid wastewater of 0.1% ~ 3% is by spraying to esterification-extraction tower 2 through atomizer spray equipment 5 after formic acid wastewater preheating pipe 1 and formic acid wastewater interchanger 15 preheating containing massfraction, the epimere of esterification-extraction tower arranges packing layer 3, middle part passes into raw steam heating alcohol by steam-heated pipe line 13, enhance esterification speed, after heating, alcohol temperature remains on 85 ~ 110 DEG C, and the spray flux of atomizer spray equipment 5 is 10 ~ 50m
3/ (m
2h), droplet moves downward under gravity and distributes at packing layer 3 inner homogeneous of esterification-extraction tower 2, spray flux according to device treatment scale and higher alcohols recoverable amount different, water-fast alcohol selected by higher alcohols, comprise propyl carbinol, Pentyl alcohol or primary isoamyl alcohol etc., the add-on of higher alcohols is determined according to tower diameter size, generally account for tower body long-pending 1/2 ~ 2/3 between, the complete submerged carriers layer (3) of general needs, formic acid wastewater droplet is dispersed in filler, after slowly entering higher alcohols liquid internal, sedimentation downwards under gravity, water droplet moves to bottom oil reservoir from entering top of oil horizon, 120s is not less than duration of contact with higher alcohols, in this process, water droplet is heated rapidly by alcohol, formic acid in water droplet and surrounding alcohol enter oil phase after fully contacting and esterification occurring, because formic acid wastewater spray flux is much smaller than the alcohol amount in tower, so can be heated rapidly in tower, simultaneously because the amount of alcohol is much larger than amount of formic acid, promote positive reaction balanced sequence, accelerate esterification reaction rate,
The object of the formic acid wastewater preheating described in present invention process is not only to promote formic acid wastewater inlet temperature of stabilizer, main object is formic acid wastewater temperature after reduction esterification-extraction tower bottom treatment, wherein dissolved organic matter is made to get back to oil reservoir, reduce organic content in the rear formic acid wastewater of purification, formic acid wastewater atomizing spray object is also not only to make formic acid fully contact with tower medium high carbon alcohol, heated rapidly, reached the temperature needed for esterification; Especially in order to formic acid in waste water fully contacts with alcohols, enable part formic acid be dissolved in alcohol, reach the object of extraction.
(2) formic acid wastewater after process is from the extraction of esterification-extraction tower 2 bottom aqueous layer 12, produced quantity approximates atomisation unit spray flux, the formic acid wastewater of bottom extraction wherein formic acid content, can by waste water extraction pipeline 14 directly discharge or discharge after simple biochemical treatment lower than 0.05%;
The object of preheating that processed waste water described in present invention process is used for initial formic acid wastewater is the heat in order to make full use of in extraction formic acid wastewater, improve the temperature that the initial formic acid wastewater of formic acid enters esterification-extraction tower, make it reach rapidly temperature needed for esterification, thus reduce the energy consumption of a whole set for the treatment of system.
(3) esterification-extraction tower 2 mesonexine oil 4 passes through pump 6 extraction to separation column 7, main containing higher alcohols, ester class and minute quantity formic acid in oily mater, by the rectifying of oil reservoir liquid pressure-reducing in tower 7, ester can be separated with alcohol, after rectifying, ester class is through piping 8 extraction, alcohol at the bottom of tower is delivered to esterification-extraction tower 2 by pipeline 9 and is recycled, and continues on for esterification extraction process, and the alcohol of middle loss supplements by mending alcohol pipeline 10.
Be the Ester of formic acid esterification gained through the material of extraction pipeline 8 extraction in present invention process, at the bottom of tower higher alcohols can continue on for esterification in esterification-extraction tower 2, object is to make its recycle, cost-saving, increases economic efficiency.
Accompanying drawing explanation
Fig. 1 is the process schematic representation of lower concentration formic acid wastewater of the present invention process, wherein: 1-formic acid wastewater preheating pipe; 2-esterification-extraction tower; 3-packing layer; 4-oil reservoir; 5-spray equipment; 6-oil reservoir extraction pump; 7-separation column; 8-ester class extraction pipeline; 9-alcohol circulating line; 10-mends alcohol pipeline; 11-formic acid wastewater transport pipe; 12-water layer; 13-steam-heated pipe line; Waste water extraction pipeline after 14-purification; 15-formic acid wastewater interchanger.
Embodiment
Below by embodiment, the present invention is specifically described, but the restriction to scope of patent protection of the present invention can not be interpreted as.
Embodiment 1:
(1) spray to esterification-extraction tower 2 by the lower concentration formic acid wastewater containing 1% by atomizing sprayer 5, tower diameter 0.8m, tower height 6m, spray flux is 50m
3/ (m
2h), make it move downward under gravity and distribute at packing layer 3 inner homogeneous, in esterification-extraction tower 2, hypomere is propyl carbinol, and volume is 1.8m
3, pipeline 13 passes into steam heating propyl carbinol, and n-butanol layer temperature is 85 DEG C.Formic acid wastewater droplet is dispersed in filler, slowly enter lower floor's propyl carbinol liquid internal, sedimentation downwards under gravity, water-oil phase is about 150s abundant duration of contact, because formic acid wastewater spray flux is very little relative to the recoverable amount of tower bottom propyl carbinol in this process, water droplet is heated rapidly; The recoverable amount of propyl carbinol is greatly excessive relative to amount of formic acid, promotes positive reaction balanced sequence, accelerates esterification reaction rate.
(2) question response stablizes the formic acid wastewater after rear esterification-extraction tower tower 2 bottom aqueous layer 12 process by formic acid wastewater in interchanger 15 preheating pipe 1, after heat exchange, water temperature drop 12 DEG C, wherein formic acid content is 0.04%, then from pipeline 14 extraction, biochemistry pool process is delivered to.After process, formic acid wastewater produced quantity equals atomisation unit spray flux, is about 6m
3/ h, in pipeline 1, after formic acid wastewater preheating, water temperature is 52 DEG C, is then delivered to tower top spray by pipeline 11.
(3) when question response is stablized by esterification-extraction tower 2 mesonexine oil 4 by pump 6 extraction to separation column 7, main containing butanols, ester class and minute quantity formic acid in oily mater, in separation column 7, oil reservoir liquid pressure-reducing is distilled, alcohol ester can be separated with formic acid, after distillation, ester class is through piping 8 extraction, propyl carbinol at the bottom of tower is delivered to esterification-extraction tower 2 by pipeline 9 and is recycled, and continues on for esterification extraction process.
Embodiment 2:
(1) spray to esterification-extraction tower 2 by the formic acid wastewater containing 0.1% by atomizing sprayer 5, tower diameter 0.9m, tower height 8m, spray flux is 15m
3/ (m
2h), make it move downward under gravity and distribute at packing layer 3 inner homogeneous of esterification-extraction tower 2, in tower 2, hypomere is primary isoamyl alcohol, and recoverable amount is 3.2m
3, pipeline 13 passes into steam heating primary isoamyl alcohol, and primary isoamyl alcohol phase temperature is 105 DEG C.Formic acid wastewater droplet is dispersed in filler, slowly enter lower floor's higher alcohols liquid internal, under gravity sedimentation downwards, water-oil phase is about 135s abundant duration of contact, because formic acid wastewater spray flux is very little relative to the recoverable amount of tower bottom alcohol in this process, water droplet is heated rapidly; The recoverable amount of alcohol is greatly excessive relative to amount of formic acid, promotes positive reaction balanced sequence, accelerates esterification reaction rate.
(2) question response stablize rear esterification-extraction tower 2 bottom aqueous layer 12 process after formic acid wastewater by formic acid wastewater in interchanger 15 preheating pipe 1, after heat exchange, formic acid wastewater temperature after process declines 8 DEG C, wherein formic acid content is 0.01%, then from pipeline 14 extraction, discharge after being delivered to biochemistry pool simple process.After process, formic acid wastewater produced quantity equals atomisation unit spray flux, is about 6m
3/ h, in pipeline 1, after formic acid wastewater preheating, water temperature is 46 DEG C, is then delivered to tower top spray by pipeline 11.
(3) when question response is stablized by esterification-extraction tower 2 mesonexine oil 4 by pump 6 extraction to separation column 7, main containing primary isoamyl alcohol, ester class and minute quantity formic acid in oily mater, by the rectifying of oil reservoir liquid pressure-reducing in separation column 7, ester can be separated with alcohol, after rectifying, ester class is through piping 8 extraction, bottom separation column 7, primary isoamyl alcohol is delivered to esterification-extraction tower 2 by pipeline 9 and is recycled, and continues on for esterification extraction process.
Embodiment 3:
(1) spray to esterification-extraction tower 2 by the lower concentration formic acid wastewater containing 2% by atomizing sprayer 5, tower diameter 1.0m, tower height 7m, spray flux is 12m
3/ (m
2h), make it move downward under gravity and distribute at packing layer 3 inner homogeneous, in esterification-extraction tower 2, hypomere is Pentyl alcohol, and recoverable amount is 6m
3, pipeline 13 passes into steam heating Pentyl alcohol, keeps Pentyl alcohol 105 DEG C mutually.Formic acid wastewater droplet is dispersed in filler, slowly enter lower floor's higher alcohols liquid internal, under gravity sedimentation downwards, water-oil phase is about 140s abundant duration of contact, because formic acid wastewater spray flux is very little relative to the recoverable amount of tower bottom alcohol in this process, water droplet is heated rapidly; The recoverable amount of alcohol is greatly excessive relative to amount of formic acid, promotes positive reaction balanced sequence, accelerates esterification reaction rate.
(2) question response stablize rear tower 2 bottom aqueous layer 12 process after formic acid wastewater by formic acid wastewater in interchanger 15 preheating pipe 1, after heat exchange, the formic acid wastewater temperature after process declines 8 DEG C, and wherein formic acid content is 0.04%, then from pipeline 14 extraction, discharge after being delivered to biochemistry pool simple process.After process, formic acid wastewater produced quantity equals atomisation unit spray flux, is about 9.5m
3/ h, in pipeline 1, after formic acid wastewater preheating, water temperature is 45 DEG C, is then delivered to tower top spray by pipeline 11.
(3) when question response is stablized by esterification-extraction tower 2 mesonexine oil 4 by pump 6 extraction to separation column 7, main containing Pentyl alcohol, ester class and minute quantity formic acid in oily mater, in separation column 7, oil reservoir liquid pressure-reducing is distilled, alcohol ester can be separated with formic acid, after distillation, ester class is through piping 8 extraction, Fractionator Bottom Pentyl alcohol is delivered to esterification-extraction tower 2 by pipeline 9 and is recycled, and continues on for esterification extraction process.
Embodiment 4:
(1) spray to esterification-extraction tower 2 by the lower concentration formic acid wastewater containing 3% by atomizing sprayer 5, tower diameter 0.85m, tower height 6.5m, spray flux is 12m
3/ (m
2h), make it move downward under gravity and distribute at packing layer 3 inner homogeneous, in esterification-extraction tower tower 2, hypomere is propyl carbinol, and recoverable amount is 2.6m
3, pipeline 13 passes into steam heating propyl carbinol, and propyl carbinol phase temperature is 85 DEG C.Formic acid wastewater droplet is dispersed in filler, slowly enter lower floor's higher alcohols liquid internal, under gravity sedimentation downwards, water-oil phase is about 140s abundant duration of contact, because formic acid wastewater spray flux is very little relative to the recoverable amount of tower bottom alcohol in this process, water droplet is heated rapidly; The recoverable amount of alcohol is greatly excessive relative to amount of formic acid, promotes positive reaction balanced sequence, accelerates esterification reaction rate.
(2) question response stablize rear tower 2 bottom aqueous layer 12 process after formic acid wastewater by formic acid wastewater in interchanger 15 preheating pipe 1, after heat exchange, the formic acid wastewater temperature after process declines 8 DEG C, and wherein formic acid content is 0.05%, then from pipeline 14 extraction, discharge after being delivered to biochemistry pool simple process.After process, formic acid wastewater produced quantity equals atomisation unit spray flux, is about 6.7m
3/ h, in pipeline 1, after formic acid wastewater preheating, water temperature is 48 DEG C, is then delivered to tower top spray by pipeline 11.
(3) when question response is stablized by esterification-extraction tower 2 mesonexine oil 4 by pump 6 extraction to separation column 7, main containing propyl carbinol, ester class and minute quantity formic acid in oily mater, in separation column 7, oil reservoir liquid pressure-reducing is distilled, alcohol, ester can be separated with formic acid, after distillation, ester class is through piping 8 extraction, Fractionator Bottom alcohol is delivered to esterification-extraction tower 2 by pipeline 9 and is recycled, and continues on for esterification extraction process.
Claims (2)
1. a treatment process for lower concentration formic acid wastewater, comprises the following steps:
(1) will be that the lower concentration formic acid wastewater of 0.1% ~ 3% is by spraying to esterification-extraction tower (2) through atomizer spray equipment (5) after preheating pipe (1) and formic acid wastewater interchanger (15) preheating containing massfraction, the epimere of esterification-extraction tower arranges packing layer (3), middle part passes into raw steam heating alcohol by steam-heated pipe line (13), enhance esterification speed, after heating, alcohol temperature remains on 85 ~ 110 DEG C, and the spray flux of atomizer spray equipment (5) is 10 ~ 50m
3/ (m
2h), droplet moves downward under gravity and packing layer (3) inner homogeneous in esterification-extraction tower (2) distributes, spray flux according to device treatment scale and higher alcohols recoverable amount different, water-fast alcohol selected by higher alcohols, the add-on of higher alcohols is determined according to tower diameter size, should account for tower body long-pending 1/2 ~ 2/3 between, need complete submerged carriers layer (3), formic acid wastewater droplet is dispersed in filler, after slowly entering higher alcohols liquid internal, sedimentation downwards under gravity, water droplet moves to bottom oil reservoir from entering top of oil horizon, 120s is not less than duration of contact with higher alcohols, in this process, water droplet is heated rapidly by alcohol, formic acid in water droplet and surrounding alcohol enter oil phase after fully contacting and esterification occurring, because formic acid wastewater spray flux is much smaller than the alcohol amount in tower, so can be heated rapidly in tower, simultaneously because the amount of alcohol is much larger than amount of formic acid, promote positive reaction balanced sequence, accelerate esterification reaction rate,
(2) formic acid wastewater after process is from esterification-extraction tower (2) bottom aqueous layer (12) extraction, produced quantity equals atomisation unit spray flux, the formic acid wastewater of bottom extraction wherein formic acid content lower than 0.05%, by waste water extraction pipeline (14) directly discharge or discharge after simple biochemical treatment;
(3) esterification-extraction tower (2) mesonexine oil (4) by pump (6) extraction to separation column (7), main containing higher alcohols, ester class and minute quantity formic acid in oily mater, by the rectifying of oil reservoir liquid pressure-reducing in separation column (7), ester is separated with alcohol, after rectifying, ester class is through piping (8) extraction, alcohol at the bottom of separation column tower is delivered to esterification-extraction tower (2) by pipeline (9) and is recycled, continue on for esterification extraction process, the alcohol of loss in the middle of process supplements by mending alcohol pipeline (10).
2. the treatment process of lower concentration formic acid wastewater according to claim 1, is characterized in that: described higher alcohols are the one in propyl carbinol, Pentyl alcohol, primary isoamyl alcohol.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3983010A (en) * | 1974-02-15 | 1976-09-28 | Basf Aktiengesellschaft | Recovery of the formic acid/water azeotrope by distillation |
| CN1354139A (en) * | 2000-11-16 | 2002-06-19 | 亚新技术株式会社 | Method and device for treating waste water containing acetic acid |
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2014
- 2014-03-19 CN CN201410102355.1A patent/CN103803691B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3983010A (en) * | 1974-02-15 | 1976-09-28 | Basf Aktiengesellschaft | Recovery of the formic acid/water azeotrope by distillation |
| CN1354139A (en) * | 2000-11-16 | 2002-06-19 | 亚新技术株式会社 | Method and device for treating waste water containing acetic acid |
Non-Patent Citations (1)
| Title |
|---|
| 从环己醇和环己酮甲酸废水中回收甲酸酯;张晓娟 等;《沈阳工业大学学报》;20081231;第30卷(第6期);第716页第1栏，第717页第1.2-1.3节，第718页第2.2节，第719页图1 * |
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