CN112239297B - Method for preparing carbon source supplement from wine wastewater and application - Google Patents
Method for preparing carbon source supplement from wine wastewater and application Download PDFInfo
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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Abstract
The invention provides a method for preparing a carbon source supplement from alcoholic wastewater and application thereof, and belongs to the technical field of water treatment. The preparation method comprises the following steps: filtering or centrifuging the liquor wastewater stock solution, and filtering by a nanofiltration membrane to obtain clear liquid 1 and concentrated liquid 1; filtering the clear liquid 1 through a reverse osmosis membrane to obtain clear liquid 2 and concentrated liquid 2; and (3) separating the concentrated solution 1 or the concentrated solution 2 through distillation to obtain tower bottom liquid which is the novel carbon source supplement. According to the method for preparing the carbon source supplement from the alcoholic wastewater, the alcoholic wastewater is used as a raw material, and after being treated by the nanofiltration membrane and the reverse osmosis membrane, the novel carbon source supplement can be obtained by rectification treatment, and the method is simple to operate and does not produce secondary pollution; the COD of the novel carbon source supplement is 30 ten thousand as a whole, can be directly used for the carbon source supplement, has low sewage treatment dosage and high denitrification efficiency, thereby greatly reducing the cost of sewage treatment plants and having popularization and application values in the treatment process of urban sewage and industrial wastewater.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a method for preparing a carbon source supplement from alcoholic wastewater and application thereof.
Background
Along with the increasing environmental protection force of the country and the gradual improvement of the sewage discharge standard, the total nitrogen index requirement is higher and higher, the general requirement reaches the first grade A standard of urban sewage discharge, namely TN <15mg/L, and the discharge standard in some areas with high environmental protection requirement is TN <10mg/L. The denitrification treatment of sewage treatment has higher requirements, and the existing denitrification treatment often has the problem of insufficient carbon sources, and the carbon sources such as sodium acetate, acetic acid, methanol, ethanol, glucose and the like must be additionally added. Acetic acid, methanol and ethanol are hazardous chemicals, and are rarely adopted for safety reasons; glucose is rarely used due to its slow denitrification rate. Sodium acetate is widely used due to high denitrification rate, wide sources and safe use, and has the main problems of high use cost and uneconomical use.
The brewing enterprises generate a great amount of brewing byproducts such as yellow water, waste lees, wine tails and the like each year. According to measurement, the pH value of the waste is=3.0-3.5, and the COD is=20000-40000 mg/L, if the waste is directly discharged without high-efficiency recycling, the waste is not only polluted and difficult to treat, but also extremely wastes resources, and the sustainable circular economy of the brewing industry is seriously restricted.
Disclosure of Invention
In view of the above, the present invention aims to provide a novel composite carbon source supplement, and a preparation method and application thereof.
Through researches, the invention adopts the following technical scheme:
1. a method for preparing a carbon source supplement from wine wastewater, comprising the following steps:
filtering or centrifuging the liquor wastewater stock solution, filtering by a nanofiltration membrane, and respectively obtaining clear liquid 1 and concentrated liquid 1 under the cross flow and tangential flow of the membrane surface;
filtering the clear liquid 1 by a reverse osmosis membrane, and respectively obtaining clear liquid 2 and concentrated liquid 2 under the cross flow and tangential flow of the membrane surface;
and (3) distilling and separating the concentrated solution 1 or the concentrated solution 2 through a rectifying tower to obtain tower bottom liquid which is the novel carbon source supplement.
Preferably, the alcoholic wastewater comprises strong aromatic yellow water, soy sauce aromatic yellow water or comprehensive wastewater.
Preferably, the nanofiltration membrane and the reverse osmosis membrane are cleaned by adopting a sodium hydroxide solution with the pH value of 10-11 before filtration. After the nanofiltration membrane and the reverse osmosis membrane are cleaned, water is used for leakage test and pressure test under the condition that the pressure is 1.5MPa, then the stock solution with impurities removed is added into a tank body, a discharging valve is opened, the emptying is carried out, and a pump is started, so that the material circulation is stable.
Preferably, the pressure of the nanofiltration membrane and the reverse osmosis membrane circulation pipeline outlet valve is 1.45-1.55 MPa. When the pressure is less than 1.5Mpa and almost no clear liquid is discharged, the pressure is slowly released, and the pump is stopped.
The alcoholic wastewater is effectively separated through an organic membrane (nanofiltration membrane and reverse osmosis membrane) to obtain concentrated liquor and clear liquor, so that preliminary enrichment is achieved.
Organic membrane separation mechanism: the solution system is separated by cross-flow and tangential flow on the membrane surface under pressure driving. Solvents (water) and other small molecule solutes pass through the microporous membrane and large molecule solutes or particles are trapped on the membrane surface by the membrane. Different rejection rates and recovery rates are caused by membrane pore size, pressure and flux differences.
Preferably, the rectification column is required to pump negative pressure to the rectification column system by a vacuum pump before distillation.
Preferably, the negative pressure value is-0.093 to-0.099 MPa.
Preferably, in the distillation separation process of the rectifying tower, the temperature of the tower bottom is 100 ℃.
Preferably, after the rectifying tower needs to carry out total reflux for 0.5h, reflux and extraction are carried out under the conditions that the temperature of the tower top is 35-37 ℃ and the reflux ratio is 8:6.
The specific steps of the operation of the rectifying tower are as follows: (1) Sucking the materials into a tower kettle (the feeding amount is 5L) under the negative pressure condition, and ensuring that the materials are free of solid impurities; (2) Starting a vacuum water pump, pumping negative pressure (gauge pressure-0.096 MPa) to a rectifying tower system, setting the heating temperature of a tower kettle to 100 ℃, and starting condensed water; (3) When materials are refluxed on the tower top, the reflux ratio is adjusted to be manual, the total reflux is performed for half an hour, and when the temperature of the tower top is stabilized at 35-37 ℃, the reflux ratio is adjusted to be automatically performed with reflux and extraction (the reflux ratio is 8:6); (4) When the liquid level of the extraction tank reaches the designated liquid level (the designated liquid level is 3.6L), stopping rectification, decompressing and cooling, discharging the kettle liquid and the materials of the extraction tank respectively, metering, sampling and testing COD.
Rectification principle: under a certain pressure, the light components (components with lower boiling points or higher saturated vapor pressures) are vaporized by utilizing the difference of the boiling points or saturated vapor pressures of the components of the miscible liquid mixture, and the concentration of the light components in the gas phase and the concentration of the heavy components in the liquid phase are gradually increased through multiple times of partial liquid phase vaporization and partial gas phase condensation, so that separation is realized.
2. The novel carbon source supplement is prepared by the method for preparing the carbon source supplement from the alcoholic wastewater.
3. The novel carbon source supplement prepared by the method for preparing the carbon source supplement from the alcoholic wastewater is applied to urban sewage and industrial wastewater treatment.
By taking a luzhou winery as an example, 100 tons of alcoholic wastewater are produced in daily life, the disposal cost is 75 yuan/t (COD 8000-15000 mg/L), the disposal cost of the alcoholic wastewater reaches 225 ten thousand yuan in one year, and the implementation of the project not only saves the disposal cost of the alcoholic wastewater, but also can recycle the alcoholic wastewater, changes waste into valuable, and has good environmental benefit.
The invention has the beneficial effects that:
1) According to the method for preparing the carbon source supplement from the alcoholic wastewater, the alcoholic wastewater is used as a raw material, and after being treated by the nanofiltration membrane and the reverse osmosis membrane, the novel carbon source supplement can be obtained by rectifying the alcoholic wastewater, and the generated wastewater can directly enter a sewage treatment device for treatment, so that the operation process is simple, no secondary pollution is generated, and the recycling value of the wastewater of a winery is greatly improved;
2) The novel carbon source supplement prepared by the method for preparing the carbon source supplement from the wine wastewater has the COD of 30 ten thousand, can be directly used for the carbon source supplement, does not need to be treated again, and is convenient and simple;
3) The novel carbon source supplement prepared by the method for preparing the carbon source supplement from the alcoholic wastewater is low in wastewater treatment dosage and high in denitrification efficiency, so that the cost of a sewage treatment plant is greatly reduced, and the method has popularization and application values in the treatment process of urban wastewater and industrial wastewater.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The method for preparing the carbon source supplement by using the alcoholic wastewater in the embodiment comprises the following steps:
pretreatment of liquor wastewater stock solution: filtering or centrifuging the stock solution to remove solid impurities and prevent the membrane from being blocked;
nanofiltration membrane treatment stock solution: preparing sodium hydroxide solution with pH of 10-11 by using sodium hydroxide to clean the nanofiltration membrane; performing leakage test and pressure test with water under the pressure of 1.5 Mpa; adding the stock solution with the impurities removed into a tank body, opening a discharging valve, evacuating, starting a pump, and stabilizing the material circulation; regulating the outlet valve of the circulating pipeline to prepare for pressure of about 1.5 Mpa; regulating the stable pressure of the circulating outlet valve to be 1.5Mpa, slowly releasing pressure and stopping the pump when the pressure is less than 1.5Mpa and almost no clear liquid is discharged; obtaining concentrated solution 1 and clear solution 1, carrying out material balance and measuring related indexes;
clear liquid 1 is treated by reverse osmosis membrane: preparing sodium hydroxide solution with pH of 10-11 by using sodium hydroxide to clean the reverse osmosis membrane; performing leakage test and pressure test with water under the pressure of 1.5 Mpa; adding the stock solution with the impurities removed into a tank body, opening a discharging valve, evacuating, starting a pump, and stabilizing the material circulation; regulating the outlet valve of the circulating pipeline to prepare for pressure of about 1.5 Mpa; regulating the stable pressure of the circulating outlet valve to be 1.5Mpa, slowly releasing pressure and stopping the pump when the pressure is less than 1.5Mpa and almost no clear liquid is discharged; obtaining concentrated solution 2 and clear solution 2, carrying out material balance and measuring related indexes;
rectifying tower processes concentrate 1 or concentrate 2: sucking the materials into a tower kettle (the feeding amount is 5L) under the negative pressure condition, and ensuring that the materials are free of solid impurities; starting a vacuum water pump, pumping negative pressure (gauge pressure-0.096 MPa) to a rectifying tower system, setting the heating temperature of a tower kettle to 100 ℃, and starting condensed water; when materials are refluxed on the tower top, the reflux ratio is adjusted to be manual, the total reflux is performed for half an hour, and when the temperature of the tower top is stabilized at 35-37 ℃, the reflux ratio is adjusted to be automatically performed with reflux and extraction (the reflux ratio is 8:6); when the liquid level of the extraction tank reaches the appointed liquid level (the appointed liquid level is 3.6L), stopping rectifying, decompressing and cooling, discharging the kettle liquid and the materials of the extraction tank respectively, metering, sampling and testing COD, wherein the kettle liquid is the novel carbon source supplement.
After the liquor wastewater stock solutions with different COD values were treated by the steps in example 1, COD detection was performed on the stock solutions, the concentrated solutions and the clear solutions at different treatment stages, and the prepared novel carbon source supplements, and the results are shown in Table 1, table 2 and Table 3.
TABLE 1 detection results of organic Membrane separation of wines and wastewater
As can be seen from table 1: (1) The organic membrane is adopted to treat the wine wastewater, so that the concentration liquid has a good enrichment effect on the COD value of the concentrated liquid, the concentration liquid is basically the liquid holdup of the equipment according to the volume quantity of the raw liquid and the initial COD value, the higher the volume quantity of the raw liquid is, the higher the initial COD value is, the enrichment effect is better, the COD value of the reverse osmosis clear liquid is about 5000, and the reverse osmosis clear liquid can be directly fed into a sewage treatment device for treatment. The COD value of the nanofiltration concentrated solution is up to about 30 ten thousand, and the nanofiltration concentrated solution can be directly used as a carbon source supplement;
(2) In the reverse osmosis membrane separation process, the COD value of the concentrated solution is generally more than 12 ten thousand, but the COD of the concentrated solution is about 8 ten thousand at the lowest, and the enrichment effect of the concentrated solution can be influenced by the following factors: firstly, after the COD value of the concentrated solution is increased, the viscosity of the liquid is increased, and substances with large molecular weight can block the pore diameter of the membrane, so that the passing rate is reduced, and the enrichment effect is affected; secondly, the membrane runs for a long time, the temperature rises, the pressure drops, the processing capacity of the membrane also drops, and the enrichment effect is affected.
TABLE 2 detection results of organic film separation of alcoholic waste water and concentration
From the rectification results in table 2, it can be seen that: (1) The nano-filtration concentrated solution with high COD can be rectified to obtain tower bottom solution with COD of more than 50 ten thousand, and the tower bottom solution can be directly used as a carbon source supplement; the COD of the tower bottom distilled by reverse osmosis reaches about 30 ten thousand, the tower bottom distilled by reverse osmosis can also be used as a carbon source supplement, the COD of the tower top produced liquid is about 5000, and the produced liquid can directly enter a sewage device for treatment;
(2) The nano-filtration and reverse osmosis concentrated liquor COD are lost in the rectification process, particularly the nano-filtration concentrated liquor loss is larger and reaches about 10 ten thousand, firstly, the tower kettle is not stirred, the materials in the tower kettle are heated unevenly, the high temperature carbonizes the organic matters, the cokes are generated on the wall of the tower kettle, and secondly, the low boiling point organic matters are not condensed, so that the COD loss is serious.
The COD obtained above was about 35 ten thousand (i.e. the bottom liquid of the reverse osmosis concentrate with the number 2 in Table 2) and about 57 Mo Zuo (i.e. the bottom liquid of the nanofiltration concentrate with the number 1 in Table 2), respectively, were subjected to denitrification treatment with a conventional carbon source (sodium acetate). The method comprises the following steps: uniformly stirring sewage from an anoxic tank of a sewage treatment plant, respectively filling the sewage into 3 1L conical flasks, adding calcium nitrate to regulate the initial total nitrogen concentration, adding different carbon sources into each conical flask, and detecting the initial total nitrogen concentration and the total nitrogen concentration of denitrification for different times; by measuring TN, NO, starting in the mother liquor mixture 3 - -N concentration and MLSS, and determining TN and NO in the system at intervals of a certain period of time 3 - The concentration of the-N can obtain TN and NO according to the determination result 3 - The removal rate of N concentration with time is obtained by adding C/delta N (the ratio of COD of the added carbon source to TN reduction after blank deduction) and the denitrification rate (the ratio mgTN/gMLSS of time of TN reduction to MLSS after a period of time of reaction), wherein the addition amount of tower bottom liquid of the reverse osmosis concentrated solution with the sequence number 2 and tower bottom liquid of the nanofiltration concentrated solution with the sequence number 1 is 150ppm, and the addition amount of the conventional carbon source is300ppm。
The COD of the carbon source is detected by a QCOD-3F type COD determinator; the total nitrogen in the sewage is detected by an LC4-CNP multiparameter water quality rapid analyzer. The results are shown in Table 3, table 4 and Table 5.
TABLE 3 denitrification Effect of different carbon sources
As can be seen from Table 3, the denitrification effect of the novel carbon source supplement prepared from the alcoholic wastewater is superior to that of the conventional carbon source supplement on the market. Conventional carbon sources are used in greater amounts than the novel carbon source supplements, but are less effective than the novel carbon source supplements.
TABLE 4 denitrification Rate of novel carbon sources and conventional carbon sources
From the analysis in Table 4, it is found that the average denitrification rate of the conventional carbon source is relatively high at the denitrification time of 1.5 hours, but the average rate of the novel carbon source is even with or slightly higher than that of the conventional carbon source at the denitrification time of 3 hours. At present, denitrification design time is about 3 hours, so that the final denitrification effect is not affected by using the novel carbon source supplement.
TABLE 5 relationship between denitrification rate and COD of carbon source
Table 5 shows the relationship between the denitrification rate and the COD value of the carbon source, and the analysis in the table shows that the average denitrification rate of the conventional carbon source is slightly faster than that of the novel carbon source when the denitrification is carried out for 1.5 hours; when denitrification is carried out for 3 hours, the average rate is differentiated and mainly depends on the COD value of the carbon source, the average rate of denitrification and the COD value of the carbon source are close to a linear relationship, namely under the condition of the same dosage, the higher the COD value is, the faster the denitrification is.
In summary, under the same conditions, the addition amount of the novel carbon source supplement is only 2/3 of that of the conventional carbon source sodium acetate; the denitrification rate within 3h is close to that of sodium acetate; the efficiency is improved, the consumption is reduced, the comprehensive cost can be saved by more than 20%, the effective content of the novel carbon source supplement is high, the COD is as high as 50 ten thousand, the denitrification efficiency is improved, the consumption is only 2/3 of that of sodium acetate, and the consumption is greatly reduced, so that the medicament cost of a sewage treatment plant is greatly reduced.
The practical domestic sewage of a septic tank of a living community is used as test water, and A is applied 2 The O process is used for treatment, and the raw water quality index is shown in Table 6. The range of the water quality index refers to the variation range of the water quality during the test, namely, 1 water sample is taken every day to be measured and the average value is calculated.
TABLE 6 raw water quality
| Index of water quality | Range | Average value of |
| COD(mg/L) | 400～600 | 500 |
| NH 4 + -N(mg/L) | 29～46 | 37.5 |
| TN(mg/L) | 28～56 | 42 |
| TP(mg/L) | 16～26 | 21 |
| pH value of | 7.12～7.46 | 7.29 |
As can be seen from the analysis in Table 6, this domestic sewage belongs to a typical low C/N ratio domestic sewage, and the average C/N is only 2.53. In the stage 2 of the test, adding a certain amount of the novel carbon source supplement provided by the invention into the domestic sewage as an external carbon source, wherein the COD addition equivalent is 150mg/L, so that the C/N ratio of the inlet water is improved, and the denitrification performance of the system is improved; the COD of the inflow water at the stage is 352.7-422.4 mg/L, and the average value is 387.2mg/L; C/N is 4.79-6.89, and the average value is 5.94. The inoculated sludge is taken from the secondary sedimentation tank return sludge of a sewage treatment plant in a Chongqing city, and belongs to the whole-course nitrified sludge.
The analysis method adopts a national standard method; comprises COD and NH 4 + -N、NO 3 - -N、NO 2 - And N, filtering the water sample through filter paper, and analyzing and measuring. TN was measured using a MultiNC 3000 total organic carbon/total nitrogen meter.
Each test phase is subjected to sampling analysis after stable operation after system adjustment. The temperature of the water in the reactor in winter is controlled to be (22+/-1) ℃ by a temperature control device, and the temperature of the water in the reactor in summer is 23-28 ℃ of the natural water temperature. The SRT of the system is controlled to be 15-20 d by discharging mud from the bottom of the secondary sedimentation tank, and the MLSS in the reactor is (2500+/-500) mg/L. The results are shown in Table 7.
Table 7 novel carbon supplement sewage treatment test
As can be seen from table 7: the novel carbon source supplement is prepared by adding the invention into a sewage treatment device, and is used for treating COD and NH in sewage 4 + -N、NO 3 - -N、NO 2 - N has good removal rate.
It should be understood that the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited to the above-described embodiment, but may be modified or substituted for some of the features described in the above-described embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for preparing a carbon source supplement from alcoholic wastewater, comprising the steps of:
filtering or centrifuging the liquor wastewater stock solution, filtering by a nanofiltration membrane, and respectively obtaining clear liquid 1 and concentrated liquid 1 under the cross flow and tangential flow of the membrane surface;
filtering the clear liquid 1 by a reverse osmosis membrane, and respectively obtaining clear liquid 2 and concentrated liquid 2 under the cross flow and tangential flow of the membrane surface;
the pressure of the nanofiltration membrane and reverse osmosis membrane circulation pipeline outlet valve is 1.45-1.55 MPa;
distilling and separating the concentrated solution 1 or the concentrated solution 2 through a rectifying tower to obtain tower bottom liquid which is the novel carbon source supplement; the rectifying tower is required to pump negative pressure to the rectifying tower system through a vacuum pump before distillation, and the rectifying tower is required to reflux and extract under the conditions that the temperature of the tower top is 35-37 ℃ and the reflux ratio is 8:6 after total reflux is carried out for 0.5 h.
2. The method for producing a carbon source supplement according to claim 1, wherein the alcoholic waste water comprises aroma yellow water, sauce yellow water or synthetic waste water.
3. The method for preparing a carbon source supplement according to claim 1, wherein the nanofiltration membrane and the reverse osmosis membrane are washed with a sodium hydroxide solution having a pH of 10 to 11 before filtration.
4. The method for producing a carbon source supplement according to claim 1, wherein the negative pressure value is-0.093 to-0.099 MPa.
5. The method for producing a carbon source supplement according to claim 1, wherein the temperature of the column bottom is 100 ℃ during the distillation and separation in the rectifying column.
6. The novel carbon source supplement prepared by the method for preparing a carbon source supplement from alcoholic waste water according to any one of claims 1 to 5.
7. Use of the novel carbon source supplement made by the method for preparing a carbon source supplement from alcoholic waste water according to any one of claims 1 to 5 in the treatment of municipal sewage and industrial waste water.
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| CN114289446A (en) * | 2021-12-21 | 2022-04-08 | 维尔利环保科技集团股份有限公司 | Resourceful treatment method for kitchen waste |
| CN114477579A (en) * | 2022-01-24 | 2022-05-13 | 四川绵竹剑南春酒厂有限公司 | Process for treating waste liquid after production of wine seasoning liquid |
| CN114804361A (en) * | 2022-05-26 | 2022-07-29 | 广东碧之江环保能源股份有限公司 | Method for producing carbon source by using waste organic solvent |
| CN114835354A (en) * | 2022-06-30 | 2022-08-02 | 北京博泰至淳生物科技有限公司 | Recycling treatment process for brewing wastewater |
| CN115583724A (en) * | 2022-10-31 | 2023-01-10 | 清华苏州环境创新研究院 | Denitrification composite carbon source and preparation method and application thereof |
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| CN108707062A (en) * | 2018-06-08 | 2018-10-26 | 聊城市鲁西化工工程设计有限责任公司 | A kind of technique for sylvite recovery processing |
| CN110255712A (en) * | 2019-06-21 | 2019-09-20 | 江苏南大环保科技有限公司 | A kind of preparation method of denitrifying carbon source |
| CN110357251A (en) * | 2019-06-21 | 2019-10-22 | 江苏南大环保科技有限公司 | One kind being used for denitrifying NEW TYPE OF COMPOSITE carbon source, preparation method and application |
| CN111410352A (en) * | 2020-04-02 | 2020-07-14 | 四川深蓝环保科技有限公司 | System and process method for preparing carbon source from resource type urban biomass hydrothermal filtrate |
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