CN112239299A - Volume reduction treatment process for laser dye spent liquor - Google Patents
Volume reduction treatment process for laser dye spent liquor Download PDFInfo
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- CN112239299A CN112239299A CN202011252851.7A CN202011252851A CN112239299A CN 112239299 A CN112239299 A CN 112239299A CN 202011252851 A CN202011252851 A CN 202011252851A CN 112239299 A CN112239299 A CN 112239299A
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 title claims abstract description 23
- 239000000990 laser dye Substances 0.000 title claims abstract description 22
- 239000000975 dye Substances 0.000 claims abstract description 58
- 238000001179 sorption measurement Methods 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 239000002351 wastewater Substances 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000012360 testing method Methods 0.000 claims abstract description 16
- 239000002699 waste material Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003456 ion exchange resin Substances 0.000 claims description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 4
- 238000012797 qualification Methods 0.000 claims description 2
- 238000012958 reprocessing Methods 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 238000004821 distillation Methods 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 20
- 230000001476 alcoholic effect Effects 0.000 description 8
- 239000000706 filtrate Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000002071 nanotube Substances 0.000 description 6
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 4
- 239000010815 organic waste Substances 0.000 description 4
- 238000002306 biochemical method Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 238000011268 retreatment Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000011001 backwashing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012806 monitoring device Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- KIDBBTHHMJOMAU-UHFFFAOYSA-N propan-1-ol;hydrate Chemical compound O.CCCO KIDBBTHHMJOMAU-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Physical Water Treatments (AREA)
- Water Treatment By Sorption (AREA)
Abstract
本发明公开了一种激光染料失效液减容处理工艺，包括以下步骤：将染料失效液输送至染料吸附系统吸附处理，处理后的产物经检测合格后输送至精馏系统进行减容处理，精馏系统分离出的废水经测试合格后排放，其分离出的醇溶液暂存。本发明提成本低，可反复循环利用，操作简单，在实现废水达标排放的基础上，节能减排，减污增效，使其中的有机溶剂可以回收利用。本发明通过吸附精馏工艺对失效液进行分步处理，染料吸附系统去除失效液中的染料成分，去除效率大于99.9%；精馏工艺将滤液进行组分分离，分离出的废水在分析测试达标后排放，废水减容量可达原废液量的60%，组分分离后产生质量浓度为68%~72%的醇溶液经测试达标进行循环再利用。
The invention discloses a volume reduction treatment process for a laser dye failure liquid, which comprises the following steps: transporting the dye failure liquid to a dye adsorption system for adsorption treatment; The wastewater separated from the distillation system is discharged after passing the test, and the separated alcohol solution is temporarily stored. The invention has low cost, can be recycled repeatedly, is simple to operate, saves energy and reduces emissions, reduces pollution and increases efficiency on the basis of achieving standard discharge of waste water, so that the organic solvent in the invention can be recycled. In the invention, the spent liquid is treated step by step through the adsorption rectification process, the dye adsorption system removes the dye components in the spent liquid, and the removal efficiency is greater than 99.9%; After discharge, the volume of waste water can be reduced by 60% of the original waste liquid. After the components are separated, the alcohol solution with a mass concentration of 68% to 72% is tested to meet the standard for recycling.
Description
Technical Field
The invention belongs to the technical field of waste liquid treatment, and particularly relates to a volume reduction treatment process for a laser dye spent liquor.
Background
Dye lasers are lasers in which certain organic dyes are dissolved in certain solvents as active media. Under the action of high-power laser, organic dye in the dye solution is decomposed and loses characteristic activity, the dye solution needs to be replaced regularly to ensure the light-emitting efficiency and the operation stability of the laser, and the replaced invalid dye solution becomes a dye invalid solution, namely aqueous organic waste liquid.
The conventional organic waste liquid treatment method can be classified into a physical method, a chemical method and a biochemical method according to the degree of difficulty in combustion, water content and chemical composition of the organic waste liquid. Physical methods include extraction, activated carbon adsorption and the like, and the method is a novel method with high efficiency and rapid separation, but because the method has single function, ideal effect is difficult to obtain for waste liquid with complex components at one time. The chemical method mainly utilizes the action of chemical reaction to convert, separate, recover and treat pollutants in the wastewater, and mainly comprises a catalytic oxidation method, an incineration method, an electrochemical method and the like. The oxidative decomposition method can be applied to aqueous low-concentration organic waste liquid, but the treatment efficiency of the waste liquid containing more organic matters is low. The incineration method comprises burning waste liquid containing combustible substances in a combustion furnace, wherein the combustible substances are also combusted with the combustible substances in the combustion furnace under the condition of a combustion-supporting device, but NO generated by combustion2、SO2Or a harmful gas such as HCl, so that the equipment used in the incineration process must be equipped with washing equipment. The biochemical method has mature process and low operation cost, is the most widely applied method in wastewater treatment, and has wide application range and high treatment capacity for treating the high-concentration refractory organic wastewater by the biochemical method.
The laser dye spent liquor consists of dye, a decomposition product thereof and a water-containing organic solvent, the components of a target product to be treated are known, the composition is not complex, and the problem of how to treat waste liquor in a targeted, economical and effective manner is a problem to be solved in the field.
Disclosure of Invention
The invention is provided for overcoming the defects in the prior art, and aims to provide a volume reduction treatment process for a laser dye spent liquor.
The invention is realized by the following technical scheme:
a laser dye spent liquor volume reduction treatment process comprises the following steps: and conveying the dye spent liquor to a dye adsorption system for adsorption treatment, conveying the product after adsorption treatment to a rectification system for volume reduction treatment after the product is detected to be qualified, discharging the wastewater separated by the rectification system after the wastewater is detected to be qualified, and temporarily storing the separated alcohol solution.
In the technical scheme, the dye spent liquor is conveyed to the dye adsorption system through the raw material supply system.
In the technical scheme, the dye adsorption system completes the decolorization of the dye in the spent liquor by using an adsorption column which takes macroporous ion exchange resin as filler.
In the above technical solution, the device for detecting the product after adsorption treatment is a dye concentration measuring device; the dye concentration measuring device is specifically an ultraviolet visible spectrophotometer measuring system.
In the technical scheme, the qualified standard of the product after adsorption treatment is that the dye concentration range is 10-20 mug/L.
In the technical scheme, when the product after adsorption treatment is unqualified, the product is conveyed back to a dye adsorption system for retreatment.
In the technical scheme, the device for testing the wastewater separated by the rectification system is a chemical oxygen demand detector, and the test qualification standard is that the COD value is less than 500 mg/L.
In the technical scheme, the wastewater separated by the rectification system is discharged into a nano-tube pipeline after passing the test; and after the concentration detection of the alcoholic solution separated by the rectification system meets the multiplexing standard, the alcoholic solution is transported to a temporary storage tank by a feed liquid conveying system and temporarily stored for reuse.
In the technical scheme, the multiplexing standard is that the concentration range of the alcoholic solution is 68-72%.
In the technical scheme, the product entering the rectification system enters a preheater, the material is fed into the middle part of a rectification tower and rectified under the heating condition of the preheater, the temperature of the reboiler is gradually increased to 100 ℃, the reflux ratio is adjusted according to the rectification state, and after the balance of the rectification system is established, waste liquid and alcohol solution begin to be discharged.
The invention has the beneficial effects that:
the invention provides a volume reduction treatment process for a laser dye spent liquor, which has the advantages of low cost, repeated cyclic utilization and simple operation, saves energy, reduces emission, reduces pollution and improves efficiency on the basis of realizing standard discharge of waste water, and ensures that an organic solvent in the waste water can be recycled. The method comprises the steps of treating the failure liquid generated by the dye laser step by step through an adsorption-rectification process, and removing the dye components in the failure liquid through a dye adsorption system, wherein the removal efficiency is more than 99.9%; the components of the filtrate (alcohol-water solution) are separated by a rectification process, the separated wastewater can be discharged through a nano tube after reaching the standard in an analysis test, the volume reduction of the wastewater can reach 60% of the original wastewater volume, and the alcohol solution with the mass concentration of 68% -72% generated after the components are separated can be recycled after reaching the standard in the test.
Drawings
FIG. 1 is a process flow diagram of the volume reduction treatment process of the laser dye spent liquor of the present invention.
Detailed Description
In order to make the technical scheme of the invention better understood by those skilled in the art, the technical scheme of the volume reduction treatment process of the laser dye spent liquor of the invention is further described by combining the drawings in the specification and through specific implementation modes.
As shown in fig. 1, a volume reduction treatment process for a laser dye spent liquor comprises the following steps: the dye failure liquid is conveyed to the dye adsorption system through the raw material supply system for adsorption treatment, the qualified products detected by the dye concentration measuring device are conveyed to the rectification system for volume reduction treatment, and the unqualified products are fed back by the calculation program and conveyed back to the dye adsorption system again for retreatment. The product entering the solution rectification system is rectified on the basis of the measurement of the concentration of the alcohol solution, and the separated wastewater is discharged into a nano-tube pipeline after being tested by a chemical oxygen demand detector to meet the national standard; and after the separated alcoholic solution meets the reuse standard through concentration detection, the separated alcoholic solution is transported to a temporary storage tank through a feed liquid conveying system and temporarily stored for reuse.
The raw material supply system comprises a feed liquid conveying gear pump, a mass flow meter and a pressure transmitter.
The dye adsorption system completes the decolorization of the dye in the failure liquid by using an adsorption column which takes macroporous ion exchange resin as filler.
The adsorption operation comprises the following specific steps:
filling the treated macroporous ion exchange resin into a column shell with phi 145 x 500, and packaging the column tube by using a sieve plate;
(ii) fixing the adsorption column on a preprocessor, backwashing the adsorption column from bottom to top with pure water of not less than 2BV at a flow rate of 100 ml/min;
(iii) mounting the treated adsorption column in a system rack, and connecting pipelines by using a quick plug;
(iv) starting a gear pump in the raw material supply system, feeding at a flow rate of 10L/h, and discharging the decolorized alcohol solution from a lower outlet of the adsorption column.
The dye concentration measuring device is specifically an ultraviolet-visible spectrophotometer measuring system, and the ultraviolet-visible spectrophotometer measuring system comprises an ultraviolet-visible spectrophotometer, a feeding peristaltic pump, an overflow cup, a sampling pipeline and the like.
The qualified standard of the product after adsorption treatment is that the dye concentration range is 10-20 mug/L.
And feeding the product entering the rectification system into a preheater, feeding the product into the middle part of a rectification tower under the heating condition of the preheater, rectifying the product, gradually increasing the temperature of a reboiler to 100 ℃, adjusting the reflux ratio according to the rectification state, and discharging waste liquid and alcohol solution after the balance of the rectification system is established.
The rectification treatment comprises the following specific steps:
setting the opening of the cooling circulation water valve to be 30 percent and displaying the flow rate to be 0.3m3/h；
(ii) starting the reboiler at a duty of 60% and raising the temperature at the bottom of the column to about 100 ℃;
(iii) when the temperature in the tower rises to 100 ℃, the tower top is stabilized at 98 ℃, the heating power of the tower kettle is set to be 30 percent, a reflux pump switch is opened, the reflux flow is 15L/h, and total reflux is carried out;
(iv) when the temperature in the tower is stabilized at 100 ℃ and the temperature at the top of the tower is stabilized at 90-91 ℃, opening a COD online measuring instrument, and testing the COD value at the bottom of the tower;
(v) when sampling measurement is carried out for two times continuously, and the COD at the bottom of the tower is less than 500, starting a rectification raw material pump switch, and then, automatically feeding for 10L/h; after the system is stabilized, the power of a rectification raw material pump is set to be 11 percent, the automatic feeding is carried out for 20L/h, and after the system is stabilized, the power of P103 is set to be 16 percent, and the automatic feeding is carried out for 30L/h;
(vi) when the liquid level of the reboiler is greater than 180mm, starting a residual liquid pump switch, and enabling the flow to be about 20L/h;
(vii) when the reflux drum level is >180mm, the product pump is started and the flow rate is about 8L/h.
The device for testing the wastewater separated by the rectification system is a chemical oxygen demand detector, and the qualified test standard is that the COD value is less than 500 mg/L.
The reuse standard is that the concentration range of the alcoholic solution is 68% -72%.
Example 1
Firstly, 100mg/L dye spent liquor of a 10% propanol-water system is conveyed into a dye adsorption system through a raw material supply system, filtrate after adsorption treatment is subjected to dye concentration measurement through an ultraviolet-visible spectrophotometer, calculation is performed through a calculation program, when the concentration is less than 10 mug/L, the filtrate is conveyed to a rectification system, the dye removal efficiency is calculated, if the concentration does not meet the requirement, the system program judges feedback, and the filtrate is conveyed to the dye adsorption system again for treatment. The method comprises the following steps that (1) filtrate entering a rectification system enters a preheater after propanol concentration is measured, the filtrate is fed from the middle part of a rectification tower and rectified under the heating condition of the preheater at 80 ℃, the temperature of a reboiler is gradually increased to 100 ℃, the reflux ratio is adjusted according to the rectification state, after the rectification system is balanced and established, wastewater is respectively separated from the bottom of the tower, and a propanol solution is separated from the top of the rectification system; the wastewater is measured by a chemical oxygen demand on-line analyzer, is discharged into a nano-tube pipeline on the premise of meeting the requirement that COD is less than 500mg/L in the national standard, and the wastewater which does not meet the discharge requirement is judged and fed back by a system program and is conveyed to the rectifying tower again for secondary treatment; and measuring the propanol solution to obtain the concentration of the alcohol solution, temporarily storing the alcohol solution in a temporary storage tank, and waiting for reuse.
The working principle of the invention is as follows:
in order to enable the volume reduction treatment process of the laser dye spent liquor to effectively treat the waste liquor generated by the dye laser, the invention adopts an adsorption-rectification method to carry out step-by-step treatment, and the alcohol solution meeting the reuse standard is recycled on the basis of reducing emission of partial waste water. The realization of the treatment process of the invention requires the cooperation of the raw material supply system, the dye adsorption system, the solution rectification system, the feed liquid conveying system and the analytical equipment including the dye concentration measuring device, the alcohol solution concentration measuring device and the water quality monitoring device. The dye failure liquid is conveyed to the dye adsorption system through the raw material supply system for adsorption treatment, the qualified product detected by the dye concentration measuring device is conveyed to the rectification system for volume reduction treatment, and the unqualified product is conveyed back to the dye adsorption system for retreatment. The product entering the solution rectification system is rectified on the basis of the measurement of the concentration of the alcohol solution, and the separated wastewater is discharged into a nano-tube pipeline after being tested by a chemical oxygen demand detector to meet the national standard; and after the separated alcoholic solution meets the reuse standard through concentration detection, the separated alcoholic solution is transported to a temporary storage tank through a feed liquid conveying system and temporarily stored for reuse.
The method comprises the steps of treating the failure liquid generated by the dye laser step by step through an adsorption-rectification process, and removing the dye components in the failure liquid through a dye adsorption system, wherein the removal efficiency is more than 99.9%; the components of the filtrate (alcohol-water solution) are separated by a rectification process, the separated wastewater can be discharged through a nano tube after reaching the standard in an analysis test, the volume reduction of the wastewater can reach 60% of the original wastewater volume, and the alcohol solution with the mass concentration of 68% -72% generated after the components are separated can be recycled after reaching the standard in the test.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011252851.7A CN112239299A (en) | 2020-11-11 | 2020-11-11 | Volume reduction treatment process for laser dye spent liquor |
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| CN202011252851.7A CN112239299A (en) | 2020-11-11 | 2020-11-11 | Volume reduction treatment process for laser dye spent liquor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115180754A (en) * | 2022-04-13 | 2022-10-14 | 华东理工大学 | A kind of cation laser dye failure liquid volume reduction treatment process |
| CN115321728A (en) * | 2022-04-13 | 2022-11-11 | 华东理工大学 | A kind of anion laser dye failure liquid volume reduction treatment process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5180497A (en) * | 1990-11-22 | 1993-01-19 | Sando Iron Works Co., Ltd. | Method for decolorization of waste water |
| CN102993456A (en) * | 2012-11-01 | 2013-03-27 | 浙江杭州鑫富药业股份有限公司 | Method for recycling colored PVB (Polyvinyl Butyral) |
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2020
- 2020-11-11 CN CN202011252851.7A patent/CN112239299A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5180497A (en) * | 1990-11-22 | 1993-01-19 | Sando Iron Works Co., Ltd. | Method for decolorization of waste water |
| CN102993456A (en) * | 2012-11-01 | 2013-03-27 | 浙江杭州鑫富药业股份有限公司 | Method for recycling colored PVB (Polyvinyl Butyral) |
Non-Patent Citations (1)
| Title |
|---|
| 席玉蕾: "中性染料母液丁醇回收工艺的研究", 《青岛科技大学硕士学位论文》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115180754A (en) * | 2022-04-13 | 2022-10-14 | 华东理工大学 | A kind of cation laser dye failure liquid volume reduction treatment process |
| CN115321728A (en) * | 2022-04-13 | 2022-11-11 | 华东理工大学 | A kind of anion laser dye failure liquid volume reduction treatment process |
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