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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- 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
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
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Abstract
The invention discloses a volume reduction treatment process for laser dye spent liquor, which comprises the following steps: conveying the dye spent liquor to a dye adsorption system for adsorption treatment, conveying the treated product to a rectification system for volume reduction treatment after the treated 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. The invention has low extraction cost, can be repeatedly recycled, has simple operation, saves energy, reduces emission, reduces pollution and improves efficiency on the basis of realizing standard discharge of waste water, and ensures that the organic solvent in the waste water can be recycled. The method comprises the steps of treating the failure liquid step by step through an adsorption rectification process, removing dye components in the failure liquid by a dye adsorption system, wherein the removal efficiency is more than 99.9%; the rectification process separates components of the filtrate, the separated wastewater is discharged after reaching the standard in an analysis test, the volume reduction of the wastewater can reach 60% of the original wastewater, and an alcohol solution with the mass concentration of 68% -72% is generated after the components are separated and is recycled after reaching the standard in the test.
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)
1. A laser dye spent liquor volume reduction treatment process is characterized by comprising the following steps: the method 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.
2. The laser dye spent liquor volume reduction treatment process according to claim 1, characterized in that: and the dye spent liquor is conveyed to the dye adsorption system through the raw material supply system.
3. The laser dye spent liquor volume reduction treatment process according to claim 1, characterized in that: 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.
4. The laser dye spent liquor volume reduction treatment process according to claim 1, characterized in that: 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.
5. The laser dye spent liquor volume reduction treatment process according to claim 1, characterized in that: the qualified standard of the product after adsorption treatment is that the dye concentration range is 10-20 mug/L.
6. The laser dye spent liquor volume reduction treatment process according to claim 1, characterized in that: and when the products after adsorption treatment are unqualified in detection, conveying the products back to the dye adsorption system for retreatment.
7. The laser dye spent liquor volume reduction treatment process according to claim 1, characterized in that: 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.
8. The laser dye spent liquor volume reduction treatment process according to claim 1, characterized in that: 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.
9. The laser dye spent liquor volume reduction treatment process according to claim 8, characterized in that: the reuse standard is that the concentration range of the alcoholic solution is 68% -72%.
10. The laser dye spent liquor volume reduction treatment process according to claim 1, characterized in that: 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.
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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 | Volume reduction treatment process for cation laser dye spent liquor |
| CN115321728A (en) * | 2022-04-13 | 2022-11-11 | 华东理工大学 | Volume reduction treatment process for anionic laser dye spent liquor |
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 |
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| 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 | Volume reduction treatment process for cation laser dye spent liquor |
| CN115321728A (en) * | 2022-04-13 | 2022-11-11 | 华东理工大学 | Volume reduction treatment process for anionic laser dye spent liquor |
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Application publication date: 20210119 |