CN102491581A - Advanced treatment method for production waste water of acrylic acid and ester device - Google Patents
Advanced treatment method for production waste water of acrylic acid and ester device Download PDFInfo
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Abstract
The invention discloses an advanced treatment method for production waste water of an acrylic acid and ester device, belonging to the technical field of treatment of organic waste water. A combined treatment process consisting of aldehyde removing treatment, coagulating and depositing two-section pretreatment, anaerobic treatment, aerobic biological secondary treatment, ozone catalytic oxidation and active carbon advanced treatment is adopted, so that the problem of advanced treatment of the production waste water of the acrylic acid and ester device is solved, and effluent can reach a national first class discharge standard of Comprehensive Sewage Discharge Standard (GB8978-96). In the combined process, biological treatment is taken as a main body, so that treatment cost on waste device of the acrylic acid and ester device can be reduced greatly.
Description
Technical field
The present invention relates to the treatment of Organic Wastewater field, relate in particular to the deep treatment method of a kind of vinylformic acid and ester apparatus factory effluent.
Background technology
Vinylformic acid and ester apparatus factory effluent are a kind of high-concentration organic industrial waste waters, chemical oxygen demand (COD
Cr) be generally 30000-50000mg/L; Be strongly-acid, mainly contain acetic acid (3.0-6.0%), vinylformic acid and ester apparatus (0.02-3.0%), formaldehyde (0.04-4%), other organism such as toluene (0-2%); Have a large amount of difficult degradations and hazardous contaminant, intractability is very big.Reported method mainly contains advanced oxidization method (burning method and catalytic wet oxidation method), component way of recycling (membrane separation process) and biological degradation mode (biological process, electrolytic-biological combined method, stripping-life assemblage method) at present.
Advanced oxidization method is handled vinylformic acid and ester apparatus waste water comprises burning method and catalytic wet oxidation method, utilizes high temperature or hyperbaric environment condition to make pollutent that thorough mineralising take place or is degraded into the method for micromolecular compound.Burning method is the main stream approach of at present domestic and international treatment of high concentration vinylformic acid and ester apparatus factory effluent, secondly is the catalytic wet oxidation method, and above-mentioned two kinds of method treatment effects are good, but investment is big, running cost is high.
Patent CN 101269899 adopts multistage electrodialysis to separate and concentrates acetate, and concentrated phase adopts multi-stage solvent extraction-rectifying mode to reclaim acetate.Patent CN 1903738 discloses a kind of vinylformic acid and ester apparatus waste water treatment process; Adopt reverse osmosis membrane that vinylformic acid and ester apparatus waste water are separated earlier; The evolution water of per-meate side is discharged the battery limit (BL), and the organism of retentate side is sent into rectifying tower, respectively acrylic acid and ester apparatus, toluene and acetate.This method does not have the Chemicals with recovery value in need of any fuel and the recoverable wastewater, compares above-mentioned technology and has the advantage that SR is little, working cost is low.But because vinylformic acid and ester apparatus waste water complicated component and production process water quality are formed fluctuation greatly, reverse osmosis membrane is prone to stop up, and quickens film and damages, and causes the film expense very big.
In recent years, for reducing the investment and the running cost of vinylformic acid and ester apparatus production wastewater treatment, be that the treatment technology of main body receives extensive concern with the biological treatment.Patent CN 1600706 has announced the high density acrylic acid wastewater, and (COD＞30000mg/L) progressively carries out anaerobic biological treatment and aerobic biological treatment, may command water outlet COD＜100mg/L behind acidication.Consider that the acroleic acid device waste strength is high, complicated component, patent CN 1948189 and patent CN 101269899 have announced the combination treatment method of physico-chemical processes and biological process.Both common ground are through the physical chemistry means waste water to be carried out pre-treatment earlier, when removing portion C OD, improve the biodegradability of organic wastewater with difficult degradation thereby, then water outlet are diluted to proper concn and carry out biochemical treatment again.Different is that CN 1948189 adopts electrolysis mode to carry out pre-treatment, and water outlet is diluted to 2000-8000mg/L and adopts anaerobic biological treatment to remove most of organism, is converted into methane, carbonic acid gas and water, removes remaining organic substance through aerobic treatment at last; And CN 101269899 adopts multistage electrodialysis to separate and concentrate acetate; Concentrated phase adopts multi-stage solvent extraction-rectifying mode to reclaim acetate; And dilute phase (COD＜3000mg/L) adopts biochemical method to handle, and effluent quality can reach (GB8978-96) first discharge standard of country's " integrated wastewater discharge standard ".
Summary of the invention
The present invention is directed to the shortcomings and deficiencies that exist in the prior art; Concrete, complicated component high to vinylformic acid and ester apparatus waste strength; Exist multiple Biostatic material (like the high density aldehydes; Especially formaldehyde), it is 150-300mg/L that the biological treatment poisonous substance of the formaldehyde of having reported allows tolerance concentration, surpasses this concentration range and will cause very big influence to the biological activity of biological treatment system.Existing biology or biology do not take into full account the restraining effect of such material to biological treatment system for the combined method of main body.The object of the invention provides the treatment process of a kind of vinylformic acid and ester apparatus factory effluent, comprise that pre-treatment, two stage biological are handled and advanced treatment three each the treatment stage.Pretreatment stage; Utilize the chemically reactive of aldehyde material that biologies such as formaldehyde inhibition aldehyde material is transformed; After its concentration is reduced to zone of reasonableness, combine coagulant precipitation to handle again, purpose is when removing portion C OD; Improve the biodegradability of waste water, improve the processing efficiency and the load of follow-up biosystem; The treatment stage of two stage biological, adopt secondary anaerobic-one-level aerobic treatment process, cooperate efficient vinylformic acid and ester engineering bacteria to carry out biological reinforced; The advanced treatment stage; Adopt catalytic ozonation-gac (security measures); The catalytic ozonation processing intent be utilize ozone again the hydroxyl radical free radical of the strong oxidation that produces down of catalyst action difficult degradation pollutent remaining in the two stage biological treat effluent is carried out oxidation or mineralising; Handle the back water outlet and can reach (GB8978-96) first discharge standard of country's " integrated wastewater discharge standard ", the activated carbon treatment unit is to preset as the security measures of technology operation exception situation.
The present invention is the deep treatment method of a kind of vinylformic acid and ester apparatus factory effluent, it is characterized in that: process step is following:
A) acrylic acid production waste water that carries out the water quality and quantity adjusting being carried out full gear handles;
B) will carry out coagulant precipitation and handle through the waste water of processing of step A;
C) waste water of step B being handled carries out secondary anaerobic to be handled;
D) waste water of step C being handled carries out the underload aerobic treatment;
E) waste water of step D being handled carries out catalytic ozonation-activated carbon treatment, and the catalytic ozonation treat effluent can reach (GB8978-96) first discharge standard of China national " integrated wastewater discharge standard ".
Like treatment process of the present invention, wherein, the full gear of steps A handle to need according to containing α-H in the waste water and the relative content that does not contain two types of aldehyde of α-H, and the full gear processing is carried out in two steps, and concrete steps are following; According to the organic aldehyde kind in vinylformic acid and the ester apparatus factory effluent; Comprise formaldehyde; The aldehyde relative content of acetaldehyde, propenal, furfural, phenyl aldehyde is divided into aldehyde and contains α-H and do not contain two types of α-H, according to the difference of the content ratio of two types of aldehyde; Adopt one or more basic metal or alkaline earth metal hydroxides additive to carry out full gear; Definite principle of its addition is following: under two types of suitable situation of aldehyde, additive is a main katalysis in reaction process, and aldehydes changes into monose compounds such as aldose and ketose; During two types of aldehyde difference great disparities, addition control reaction system is the alkaline pH scope, and additive was both participated in reaction also as catalyzer as reductive agent;
1) pending acrylic acid wastewater being carried out the total analysis of aldehyde material, serves as according to it being divided into two big types, the relative content of two types of materials of statistics whether to contain α-H; Thereby there are three kinds of situation in the acrylic acid wastewater that contains aldehyde:
A kind of be contain α-H and do not contain two big types of aldehyde total amounts of α-H suitable;
Be that two types of aldehydes exist than big-difference in addition, be respectively contain α-H in the pending acrylic acid wastewater aldehyde greater than the aldehyde that does not contain α-H; Perhaps, confirm according to Analysis Results of Water Quality which kind of situation the pending aldehyde acrylic acid wastewater that contains belongs to less than two kinds of situation of the aldehyde that does not contain α-H.
2) when the aldehyde that contains α-H in the pending acrylic acid wastewater when not containing α-H aldehyde, through alkaline earth metal hydroxides be selected from sodium hydroxide, calcium hydroxide, Pottasium Hydroxide in one or more additives; Drip gradually and the system pH of keeping is 10～13, temperature of reaction is 45-95 ℃, and the reaction times is 0.5-12h;
3) when the aldehyde that contains α-H in the pending acrylic acid wastewater when not containing the aldehyde of α-H, handle and be divided into two stages: the fs, through alkaline earth metal hydroxides; Be selected from sodium hydroxide, calcium hydroxide, Pottasium Hydroxide in one or more; Drip gradually and the system pH of keeping is 10～13, temperature of reaction is 45-95 ℃, and the reaction times is 0.5-12h; Subordinate phase detects remaining total aldehyde content, adds one or more above-mentioned alkaline earth metal hydroxidess more fast, and remaining aldehyde and alkaline earth metal hydroxides mol ratio 1: 1～3: 1, control reaction temperature are 50-95 ℃, and the reaction times is 0.5-10h;
Like treatment process of the present invention, wherein, the coagulant precipitation of step B is handled and is mixed, reacts back 1-5min with coagulating agent after the acrylic acid production waste water that will pass through the full gear processing is regulated pH value acid range, and velocity slope is controlled at 200-700S
-1In waste water, add flocculation agent reaction 10-20min again, velocity slope is 200S
-1Weaken to 20S
-1At last waste water is carried out solid-liquid separation, solid-liquid separation time 1.5-2.5h;
Like treatment process of the present invention; Wherein, Step C regulates wastewater pH to the 7.8-9.0 scope, adopts the secondary anaerobic biological treatment system, can select multiple reactor drum operation such as UASB, IC, EGSB or AF form for use; Reduce the organic concentration in the waste water significantly, reach the waste water aerobic load of processing and require (COD is 200-1000mg/L).
Like treatment process of the present invention, wherein, the aerobic treatment system of step D can adopt the operation scheme such as ASP, BAF, MBR of underload.
Like treatment process of the present invention; Wherein, Step e adopts catalytic ozonation-gac (security measures); The catalytic ozonation processing intent be utilize ozone again the hydroxyl radical free radical of the strong oxidation that produces down of catalyst action difficult degradation pollutent remaining in the two stage biological treat effluent is carried out oxidation or mineralising, ozone and waste water duration of contact are 15-240min, the ozone dosage is 30-500mg/L; Ozone adopts continuous dosing method, adds the homogeneous catalyst of O3 catalytic oxidation reaction or with Al
2O
3, SiO
2Or gac is that heterogeneous catalyst that the activating oxide of carrier loaded Cu, Fe, Mn metal is processed is handled the back water outlet and can be reached (GB8978-96) first discharge standard of country's " integrated wastewater discharge standard ", and the activated carbon treatment unit is to preset as the security measures of technology operation exception situation.
The present invention compared with prior art; Have following outstanding advantage and beneficial effect: to the formaldehyde that contains high density in vinylformic acid and the ester apparatus factory effluent; The characteristics of waste water difficult degradation; The present invention's proposition " full gear processing " solution high-concentration formaldehyde and other aldehydes are to the toxic action of mikrobe; Adopt the wastewater treatment process of " pre-treatment (processing of full gear processing-coagulant precipitation)-second-stage treatment (two-stage anaerobic-aerobe is handled)-advanced treatment (catalytic ozonation-gac) " of economical rationality; Solved the processing difficult problem of vinylformic acid and ester apparatus factory effluent, water outlet can reach (GB8978-96) first discharge standard of country's " integrated wastewater discharge standard ".Invention provides the treatment process of a kind of vinylformic acid and ester apparatus factory effluent; Take the full gear preprocessing means to reduce the total aldehyde content of organic waste water; For being that the technology of main body provides feasibility with the biological treatment; When removing portion C OD, improve the biodegradability of waste water, improve the processing efficiency and the load of follow-up biosystem.The present invention also can be applicable to vinylformic acid and ester apparatus factory effluent and waste water quality trade effluent similar with it.
Embodiment
Embodiment 1:
Table 1 between vinylformic acid that adopts in the present embodiment and ester apparatus waste water quality situation:
Table 1 vinylformic acid and ester apparatus waste water quality information slip
| pH | COD Cr | TOC | BOD 5 | B/C | Formaldehyde | Total aldehyde |
| 4.2 | 49320 | 22223 | 75 | 0.0015 | 7900 | 8573 |
At first vinylformic acid and ester apparatus waste water are carried out the full gear processing, 95 ℃ of control reaction temperature slowly add earth alkali metal (sodium hydroxide and calcium hydroxide ratio 1: 2) regulation system pH=13, reaction times 0.5h.Back water outlet dosing coagulant bodied ferric sulfate 300mg/L is handled in full gear, residence time 5min, and the G value is got 550S
-1, adding 3mg/L coagulant aids PAM, velocity slope is 200S
-1Weaken to 20S
-1, hydraulic detention time 20min, solid-liquid separation time 0.5h.Waste water is through after the pre-treatment, and control water inlet organic loading is 12.0kgCOD
Cr/ m
3D adopts the operation scheme of two-stage EGSB (the pH value is controlled at 7.8-8.3 for granule sludge character parameter 57-69gVSS/L, particle diameter 0.2-5.0mm, and temperature 18-31 ℃, upflow velocity is 5m/s, residence time 48h)-one-level MBR (residence time 18h) to handle.Through after the second-stage treatment, remaining Persistent organic pollutants are carried out the catalytic ozonation processing in the waste water, and be 120min duration of contact, and the ozone dosage is 500mg/L, and ozone adopts continuous dosing method, adds with Al
2O
3The heterogeneous catalyst of processing for the activating oxide of metals such as carrier loaded Cu, Fe, Mn.Water outlet can reach (GB8978-96) first discharge standard of country's " integrated wastewater discharge standard ".
Each cell processing effect of table 2
| Project | COD Cr | TOC | BOD 5 | B/C | Formaldehyde | Total aldehyde |
| Former water | 49320 | 22223.0 | 75 | 0.0015 | 7900 | 8573 |
| The full gear water outlet | 53493 | 21840.0 | 16782 | 0.31 | - | - |
| The coagulation water outlet | 40748 | 16637.7 | 19966 | 0.49 | ||
| Two-stage UASB water outlet | 1102 | 354.0 | 375 | 0.34 | ||
| MBR | 425 | 35.7 | 10.7 | 0.025 |
| Catalytic ozonation | 52 | 7.1 | 10.0 | 0.19 |
Embodiment 2:
Table 3 between vinylformic acid that adopts in the present embodiment and ester apparatus waste water quality situation:
Table 3 vinylformic acid and ester apparatus waste water quality information slip
| pH | COD Cr | TOC | BOD 5 | B/C | Formaldehyde | Total aldehyde |
| 3.9 | 35217 | 14972.0 | 23 | 0.0015 | 6512 | 7891 |
At first vinylformic acid and ester apparatus waste water are carried out the full gear processing, 45 ℃ of control reaction temperature slowly add earth alkali metal (sodium hydroxide and calcium hydroxide ratio 1: 2) regulation system pH=13, reaction times 12h.Back water outlet dosing coagulant bodied ferric sulfate 300mg/L is handled in full gear, residence time 5min, and the G value is got 550S
-1, adding 3mg/L coagulant aids PAM, velocity slope is 200S
-1Weaken to 20S
-1, hydraulic detention time 20min, solid-liquid separation time 0.5h.Waste water is through after the pre-treatment, and control water inlet organic loading is 4.0kgCOD
Cr/ m
3D adopts the operation scheme of two-stage UASB (the pH value is controlled at 7.8-8.3 for granule sludge character parameter 45-53gVSS/L, particle diameter 0.2-5.0mm, and temperature 18-31 ℃, upflow velocity is 4.5m/s, residence time 36h)-one-level ASP (residence time 24h) to handle.Through after the second-stage treatment, remaining Persistent organic pollutants are carried out the catalytic ozonation processing in the waste water, and be 120min duration of contact, and the ozone dosage is 300mg/L, and ozone adopts continuous dosing method, adds with Al
2O
3The heterogeneous catalyst of processing for the activating oxide of metals such as carrier loaded Cu, Fe, Mn.Water outlet can reach (GB8978-96) first discharge standard of country's " integrated wastewater discharge standard ".
Each cell processing effect of table 4
| Project | COD Cr | TOC | BOD 5 | B/C | Formaldehyde | Total aldehyde |
| Former water | 35217 | 14972.0 | 23 | 0.0015 | 6512 | 7891 |
| The full gear water outlet | 38614 | 14852.0 | 12356 | 0.32 | - | - |
| The coagulation water outlet | 29347 | 16637.1 | 13793 | 0.47 | ||
| Two-stage UASB water outlet | 1204 | 351.9 | 397 | 0.33 | ||
| ASP | 537 | 42.6 | 13.7 | 0.026 | ||
| Catalytic ozonation | 42 | 6.1 | 9.0 | 0.21 |
Claims (6)
1. the deep treatment method of vinylformic acid and ester apparatus factory effluent, it is characterized in that: process step is following:
A) acrylic acid production waste water that carries out the water quality and quantity adjusting being carried out full gear handles;
B) will carry out coagulant precipitation and handle through the waste water of processing of step A;
C) waste water of step B being handled carries out secondary anaerobic to be handled;
D) waste water of step C being handled carries out the underload aerobic treatment;
E) waste water of step D being handled carries out catalytic ozonation-activated carbon treatment, and the catalytic ozonation treat effluent can reach (GB8978-96) first discharge standard of China national " integrated wastewater discharge standard ".
2. treatment process as claimed in claim 1, wherein, the full gear of steps A handle to need according to containing α-H in the waste water and the relative content that does not contain two types of aldehyde of α-H, and the full gear processing is carried out in two steps, and concrete steps are following; According to the organic aldehyde kind in vinylformic acid and the ester apparatus factory effluent; Comprise formaldehyde; The aldehyde relative content of acetaldehyde, propenal, furfural, phenyl aldehyde is divided into aldehyde and contains α-H and do not contain two types of α-H, according to the difference of the content ratio of two types of aldehyde; Adopt one or more basic metal or alkaline earth metal hydroxides additive to carry out full gear, definite principle of its addition is following; Under two types of suitable situation of aldehyde, additive is a main katalysis in reaction process, and aldehydes changes into monose compounds such as aldose and ketose; During two types of aldehyde difference great disparities, addition control reaction system is the alkaline pH scope, and additive was both participated in reaction also as catalyzer as reductive agent;
1) pending acrylic acid wastewater being carried out the total analysis of aldehyde material, serves as according to it being divided into two big types, the relative content of two types of materials of statistics whether to contain α-H; Thereby there are three kinds of situation in the acrylic acid wastewater that contains aldehyde:
A kind of be contain α-H and do not contain two big types of aldehyde total amounts of α-H suitable;
Be that two types of aldehydes exist than big-difference in addition, be respectively contain α-H in the pending acrylic acid wastewater aldehyde greater than the aldehyde that does not contain α-H; Perhaps, confirm according to Analysis Results of Water Quality which kind of situation the pending aldehyde acrylic acid wastewater that contains belongs to less than two kinds of situation of the aldehyde that does not contain α-H.
2) when the aldehyde that contains α-H in the pending acrylic acid wastewater when not containing α-H aldehyde, through alkaline earth metal hydroxides be selected from sodium hydroxide, calcium hydroxide, Pottasium Hydroxide in one or more additives; Drip gradually and the system pH of keeping is 10～13, temperature of reaction is 45-95 ℃, and the reaction times is 0.5-12h;
3) when the aldehyde that contains α-H in the pending acrylic acid wastewater when not containing the aldehyde of α-H, handle and be divided into two stages: the fs, through alkaline earth metal hydroxides; Be selected from sodium hydroxide, calcium hydroxide, Pottasium Hydroxide in one or more; Drip gradually and the system pH of keeping is 10～13, temperature of reaction is 45-95 ℃, and the reaction times is 0.5-12h; Subordinate phase detects remaining total aldehyde content, adds one or more above-mentioned alkaline earth metal hydroxidess more fast, and remaining aldehyde and alkaline earth metal hydroxides mol ratio 1: 1～3: 1, control reaction temperature are 50-95 ℃, and the reaction times is 0.5-10h;
3. treatment process as claimed in claim 1, wherein, the coagulant precipitation of step B is handled and is mixed, reacts back 1-5min with coagulating agent after the acrylic acid production waste water that will pass through the full gear processing is regulated pH value acid range, and velocity slope is controlled at 200-700S
-1In waste water, add flocculation agent reaction 10-20min again, velocity slope is 200S
-1Weaken to 20S
-1At last waste water is carried out solid-liquid separation, solid-liquid separation time 1.5-2.5h;
4. treatment process as claimed in claim 1; Wherein, Step C regulates wastewater pH to the 7.8-9.0 scope, adopts the secondary anaerobic biological treatment system, selects UASB, IC, EGSB or many kinds of reactor drum operations of AF form for use; Reduce the organic concentration in the waste water significantly, reach the waste water aerobic load of processing and require (COD is 200-1000mg/L).
5. treatment process as claimed in claim 1, wherein, the aerobic treatment system of step D, ASP, BAF, the MBR operation scheme of employing underload.
6. treatment process as claimed in claim 1; Wherein, step e adopt catalytic ozonation-gac, catalytic ozonation processing intent be utilize ozone again the hydroxyl radical free radical of the strong oxidation that produces down of catalyst action difficult degradation pollutent remaining in the two stage biological treat effluent is carried out oxidation or mineralising; Ozone and waste water duration of contact are 15-240min; The ozone dosage is 30-500mg/L, and ozone adopts continuous dosing method, adds the homogeneous catalyst of O3 catalytic oxidation reaction or with Al
2O
3, SiO
2Or gac is that heterogeneous catalyst that the activating oxide of carrier loaded Cu, Fe, Mn metal is processed is handled the back water outlet and can be reached (GB8978-96) first discharge standard of China national " integrated wastewater discharge standard ", and the activated carbon treatment unit is to preset as the security measures of technology operation exception situation.
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| CN102976561A (en) * | 2012-12-17 | 2013-03-20 | 天津工业大学 | Technique for treating phenol/anisole-containing production wastewater |
| CN105084656A (en) * | 2015-08-10 | 2015-11-25 | 蓝星（北京）技术中心有限公司 | Treatment method for industrial waste water of methionine |
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| CN108409044A (en) * | 2018-04-04 | 2018-08-17 | 蓝星安迪苏南京有限公司 | Method and device for handling acrolein reaction device waste water |
| US11358885B2 (en) | 2018-04-04 | 2022-06-14 | Bluestar Adisseo Nanjing Co., Ltd. | Method and device for treating acrolein reactor wastewater |
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| CN109354310A (en) * | 2018-11-13 | 2019-02-19 | 江苏蓝必盛化工环保股份有限公司 | A kind of processing method of acrylic acid wastewater |
| CN109928582A (en) * | 2019-04-18 | 2019-06-25 | 南京清元景和环境科技有限公司 | Biological, the chemically composited processing method of formaldehyde-containing wastewater |
| CN110294569A (en) * | 2019-06-14 | 2019-10-01 | 江苏南大华兴环保科技股份公司 | A kind of processing method of polyurethane production waste water |
| CN111807647A (en) * | 2020-08-11 | 2020-10-23 | 苏州聚智同创环保科技有限公司 | Advanced treatment system and method for acrylic acid wastewater |
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