CN105084608A - Pretreatment method of acrylate wastewater biochemical treatment - Google Patents
Pretreatment method of acrylate wastewater biochemical treatment Download PDFInfo
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- CN105084608A CN105084608A CN201510595519.3A CN201510595519A CN105084608A CN 105084608 A CN105084608 A CN 105084608A CN 201510595519 A CN201510595519 A CN 201510595519A CN 105084608 A CN105084608 A CN 105084608A
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Abstract
The embodiment of the invention discloses a pretreatment method of acrylate wastewater biochemical treatment. COD of acrylate wastewater is 60,000-120,000 mg/L. The method comprises the steps that 1, the pH value of the acrylate wastewater is adjusted to range from 1 to 3.5 through a sulfuric acid solution; 2, a soluble calcium salt solution is added to the acrylate wastewater with the adjusted pH value, oscillation or stirring treatment is conducted for 10-60 min, solid-liquid separation treatment is conducted, and separation liquid is collected, wherein adding quantity of the soluble calcium salt solution is 0.1%-0.35% of the mass of the acrylate wastewater, and the soluble calcium salt solution is one or more of calcium chloride, calcium nitrate and calcium acetate; 3, extraction treatment is conducted on filtrate obtained in the second step, and raffinate is pretreatment effluent. According to the pretreatment method of the acrylate wastewater biochemical treatment, the process is simple, and the energy consumption is low. The biodegradability of the acrylate wastewater which is treated through the method is larger than 0.5, and biochemical treatment can be conducted directly.
Description
Technical field
The present invention relates to technical field of waste water processing, the pretreatment process of particularly a kind of acrylic ester wastewater biochemical treatment.
Background technology
Acrylic ester wastewater refers to the waste water produced acrylate and produce.Main containing pollutents such as propyl carbinol, sodium acrylate, tosic acid, sodium hydroxide in this waste water.Acrylic ester wastewater is mainly derived from processing wastewater, equipment cleaning water, irregular discharge water etc., and its water quality is complicated, hardly degraded organic substance content high (COD > 100000mg/L), and saltiness is high, difficult treatment.
When utilizing biochemical technology process acrylic ester wastewater, usually need to carry out pre-treatment to waste water, reduce organic content in acrylic ester wastewater, make the biodegradability of acrylic ester wastewater (B/C) be greater than 0.4, then carry out biochemical treatment.Present stage, the pretreatment process of acrylic ester wastewater biochemical treatment has electroosmose process, electrolytic process, all needs to consume electric energy, and in actual production, energy consumption is high.
Summary of the invention
The embodiment of the invention discloses a kind of pretreatment process of acrylic ester wastewater biochemical treatment, the problem that the pretreatment process energy consumption for solving existing acrylic ester wastewater biochemical treatment is high.Technical scheme is as follows:
A pretreatment process for acrylic ester wastewater biochemical treatment, the COD of described acrylic ester wastewater is 60000 ~ 120000mg/L, comprises the following steps:
1), with sulphuric acid soln, the pH value of acrylic ester wastewater is adjusted to 1 ~ 3.5;
2), by solubility calcium salts solution joining mixes up in the acrylic ester wastewater of pH value, vibration or stir process 10 ~ 60min, and parting liquid is collected in solid-liquid separation process; The dosage of described soluble calcium salt is 0.1% ~ 0.35% of described acrylic ester wastewater quality; Described soluble calcium salt is at least one in calcium chloride, nitrocalcite and lime acetate;
3), to step 2) filtrate that obtains carries out extraction treatment, and obtain extraction phase and extracting phase, extracting phase is pre-treatment water outlet; Extraction agent is one or more in the mixing solutions of tributyl phosphate and kerosene, benzene, toluene and hexanaphthene; Described extraction agent and step 2) volume ratio of filtrate that obtains is (0.5 ~ 2.5): 1.
In the preferred embodiment of the present invention, step 1) in sulphuric acid soln, the pH value of described acrylic ester wastewater is adjusted to 1.5 ~ 3.
In one of the present invention more preferred implementation, step 1) in sulphuric acid soln, the pH value of described acrylic ester wastewater is adjusted to 1.5 ~ 2.5.
In one of the present invention more preferred implementation, the dosage of described soluble calcium salt is 0.2% ~ 0.3% of described acrylic ester wastewater quality.
In one of the present invention more preferred implementation, described extraction agent and step 2) volume ratio of filtrate that obtains is (1 ~ 1.5): 1.
In one of the present invention more preferred implementation, described extraction agent is at least one in the mixing solutions of tributyl phosphate and kerosene, Benzene and Toluene.
In one of the present invention more preferred implementation, also comprise and reclaim vinylformic acid in extraction phase.
In the preferred embodiment of the present invention, in the mixing solutions of described tributyl phosphate and kerosene, the volume fraction of tributyl phosphate is 20% ~ 50%.
The pretreatment process technique of a kind of acrylic ester wastewater biochemical treatment provided by the invention is simple, and energy consumption is low.Biodegradability through the acrylic ester wastewater of this method process is greater than 0.49, directly can carry out biochemical treatment.
Embodiment
Technical scheme of the present invention: a kind of pretreatment process of acrylic ester wastewater biochemical treatment, the COD of described acrylic ester wastewater is 60000 ~ 120000mg/L, comprises the following steps:
1), with sulphuric acid soln, the pH value of acrylic ester wastewater is adjusted to 1 ~ 3.5;
2), by solubility calcium salts solution joining mixes up in the acrylic ester wastewater of pH value, vibration or stir process 10 ~ 60min, and parting liquid is collected in solid-liquid separation process; The dosage of described soluble calcium salt is 0.1% ~ 0.35% of described acrylic ester wastewater quality; Described soluble calcium salt is at least one in calcium chloride, nitrocalcite and lime acetate;
3), to step 2) filtrate that obtains carries out extraction treatment, and obtain extraction phase and extracting phase, extracting phase is pre-treatment water outlet; Extraction agent is one or more in the mixing solutions of tributyl phosphate and kerosene, benzene, toluene and hexanaphthene; Described extraction agent and step 2) volume ratio of filtrate that obtains is (0.5 ~ 2.5): 1.
In experimentation, contriver is surprised to find that, regulate the pH value value 1 ~ 3.5 of acrylic ester wastewater with sulphuric acid soln after, add soluble calcium salt wherein, a large amount of white precipitates can be produced, namely the calcium sulfate of water is slightly soluble in, meanwhile, suspended particle in acrylic ester wastewater and some water-fast organic substances together can precipitate with the generation of calcium sulfate, through solid-liquid separation process, collect parting liquid, then parting liquid is carried out extraction treatment, raffinate is pre-treatment water outlet, can reach the standard (biodegradability is greater than 0.4) of biochemical treatment.
It should be noted that, the process of the present invention's said solid-liquid separation can adopt the technique means such as centrifugal, filtration.Centrifugally usually be set as 1000 ~ 4000 revs/min, centrifugal 10 ~ 30min.Filtration generally includes suction filtration, husky filter, filter press etc.Solid-liquid separation is this area routine techniques means, and the present invention does not do concrete restriction at this.
In the inventive solutions, preferably, step 1) in sulphuric acid soln, the pH value of described acrylic ester wastewater is adjusted to 1.5 ~ 3, more preferably, pH value is adjusted to 1.5 ~ 2.5.
In the inventive solutions, the dosage of described soluble salt is 0.2% ~ 0.3% of described acrylic ester wastewater quality, effectively can remove the suspended particle in water and water-fast organic substance.
In the inventive solutions, described extraction agent and step 2) volume ratio of filtrate that obtains is (1 ~ 1.5): 1, can by the most of acrylic acid extraction in acrylic ester wastewater out.
In actual applications, technical scheme of the present invention can also comprise vinylformic acid in recovery extraction phase.Specifically can adopt massfraction be 20% ~ 50% NaOH solution strip obtain sodium acrylate, or to extraction phase carry out distillation process acrylic acid.According to acrylic acid boiling point, the temperature of distillation process can be 141 DEG C ~ 150 DEG C, and those skilled in the art can determine voluntarily, and the present invention does not do concrete restriction at this.In actual applications, in the mixing solutions of described tributyl phosphate and kerosene, the volume fraction of tributyl phosphate is 20% ~ 50%.
In the inventive solutions, said sulphuric acid soln is aqueous sulfuric acid.Said solubility calcium salts solution is water-soluble calcium saline solution.In actual applications, soluble calcium salt mass concentration in the solution can be 100g/L ~ 350g/L, and those skilled in the art can determine voluntarily according to practical experience, and the present invention does not do concrete restriction at this.
Be described technical scheme of the present invention below in conjunction with specific embodiment, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Reagent used by embodiment all commercially.
Embodiment 1
The Raw performance of acrylic ester wastewater: COD is 119000mg/L, pH value 13.2.
Measure 1000ml acrylic ester wastewater, regulate its pH value to 3.5 with the sulphuric acid soln that massfraction is 98%.Add the calcium chloride solution 10ml of 350g/L again, vibration 30min, suction filtration, obtains filtrate.
Add in filtrate 1500ml tributyl phosphate volume fraction be 50% tributyl phosphate and kerosene mixing solutions extract as extraction agent.At 141 DEG C, distill extraction phase, acrylic acid, extraction agent can be recycled.Raffinate is pre-treatment water outlet, and the COD of raffinate is 10590mg/L, COD clearance be 91.2%, B/C ratio is 0.58, with after acid for adjusting pH to 8.0, can directly enter anaerobic biochemical treatment system.
Embodiment 2
The Raw performance of acrylic ester wastewater: COD is 61254mg/L, pH value 2.6.
Measure 1000ml acrylic ester wastewater, regulate its pH value to 1.0 with the sulphuric acid soln that massfraction is 50%.Add the calcium chloride solution 10ml of 100g/L again, vibration 20min, suction filtration, obtains filtrate.
In filtrate, add 500ml toluene extract as extraction agent.Carry out back extraction with the 20%NaOH aqueous solution to extraction phase, acrylic acid sodium, extraction agent can be recycled.Raffinate is pre-treatment water outlet, and the COD of raffinate is 5819mg/L, COD clearance be 90.5%, B/C ratio is 0.54, with after acid for adjusting pH to 7.6, directly can enter anaerobic-aerobic bioreactor.
Embodiment 3
The Raw performance of acrylic ester wastewater: COD is 89000mg/L, pH value 8.2.
Measure 1000ml acrylic ester wastewater, regulate its pH value to 2.5 with the sulphuric acid soln that massfraction is 50%.Add the calcium acetate solution 10ml of 200g/L again, vibration 40min, suction filtration, obtains filtrate.
In filtrate, add 2000ml toluene extract as extraction agent.Carry out back extraction with the 30%NaOH aqueous solution to extraction phase, acrylic acid sodium, extraction agent can be recycled.Raffinate is pre-treatment water outlet, and the COD of raffinate is 4895mg/L, COD clearance be 94.5%, B/C ratio is 0.53, directly can enter anaerobic biological reactor.
Embodiment 4
The Raw performance of acrylic ester wastewater: COD is 102650mg/L, pH value 13.5.
Measure 1000ml acrylic ester wastewater, regulate its pH value to 3 with the sulphuric acid soln that massfraction is 50%.Add the calcium acetate solution 10ml of 300g/L again, vibration 40min, suction filtration, obtains filtrate.
In filtrate, add 2500ml cyclohexane give is that extraction agent extracts.Carry out back extraction with the 30%NaOH aqueous solution to extraction phase, acrylic acid sodium, extraction agent can be recycled.Raffinate is pre-treatment water outlet, and the COD of raffinate is 5670mg/L, COD clearance be 93.6%, B/C ratio is 0.52, directly can enter anaerobic biological reactor.
Embodiment 5
The Raw performance of acrylic ester wastewater: COD is 60100mg/L, and pH value is 13.
Measure 1000ml acrylic ester wastewater, regulate its pH value to 2 with the sulphuric acid soln that massfraction is 50%.Add the calcium acetate solution 10ml of 250g/L again, vibration 40min, suction filtration, obtains filtrate.
Add in filtrate 2500ml tributyl phosphate volume fraction be 20% tributyl phosphate and kerosene mixing solutions extract as extraction agent.At 141 DEG C, distill extraction phase, acrylic acid, extraction agent can be recycled.Raffinate is pre-treatment water outlet, and the COD of raffinate is 5109mg/L, COD clearance be 91.5%, B/C ratio is 0.56, directly can enter anaerobic biological reactor.
Comparative example 1
The Raw performance of acrylic ester wastewater: COD is 60100mg/L, pH value 13.
Getting the waste water of 1000ml containing acrylate, is the sulphur acid for adjusting pH to 2 of 50% with massfraction; Add 250g/L calcium sulfate turbid solution 10ml, vibration 40min, suction filtration, obtains filtrate.
Add in filtrate 2500mL tributyl phosphate volume fraction be 20% tributyl phosphate and kerosene mixing solutions extract as extraction agent.Raffinate is pre-treatment water outlet, and the COD of raffinate is 31072mg/L, COD clearance be 48.3%, B/C ratio is 0.28, directly can not enter biochemical system.
Comparative example 2
The Raw performance of acrylic ester wastewater: COD is 60100mg/L, pH value 13.
Get the waste water of 1000ml containing acrylate, be the sulphur acid for adjusting pH to 5.5 of 50% with massfraction, add 0.5g polymerised sulphur acidifying iron (PFS), stir 20 minutes, in solution, engender a small amount of flco, filter, obtain filtrate.
Regulate filtrate pH to 2.0 with the sulfuric acid that massfraction is 50%, add in the filtrate regulating pH 2500mL tributyl phosphate volume fraction be 20% tributyl phosphate kerosene mixing solutions extract as extraction agent.Raffinate is the COD of pre-treatment water outlet raffinate is that 27886mg/L, COD clearance reaches 53.6%, B/C of former water than 0.26, directly can not enter biochemical system.
As can be seen from comparative example 1 and 2, directly all do not reach the COD removal effect of embodiment 1 to 5 acquisition with the Polyferric Sulfate Flocculants that solution and this area of calcium sulfate preparation are commonly used.
From above-described embodiment and comparative example, the pretreatment process technique of a kind of acrylic ester wastewater biochemical treatment disclosed by the invention is simple, create beyond thought technique effect, the COD clearance of acrylic ester wastewater is more than 90%, the B/C ratio of pre-treatment water outlet is more than 0.5, reaches the standard of biochemical treatment.
It should be noted that, the said COD of the present invention refers to the chemical oxygen demand (COD) determined as oxygenant by potassium bichromate.
Above the pretreatment process of a kind of acrylic ester wastewater biochemical treatment provided by the present invention is described in detail.Apply specific embodiment herein to set forth principle of the present invention and embodiment, the explanation of above embodiment just understands method of the present invention and clou thereof for helping.It should be pointed out that for the person of ordinary skill of the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify the protection also falling into the claims in the present invention.
Claims (8)
1. a pretreatment process for acrylic ester wastewater biochemical treatment, the COD of described acrylic ester wastewater is 60000 ~ 120000mg/L, it is characterized in that, comprises the following steps:
1), with sulphuric acid soln, the pH value of acrylic ester wastewater is adjusted to 1 ~ 3.5;
2), by solubility calcium salts solution joining mixes up in the acrylic ester wastewater of pH value, vibration or stir process 10 ~ 60min, and parting liquid is collected in solid-liquid separation process; The dosage of described soluble calcium salt is 0.1% ~ 0.35% of described acrylic ester wastewater quality; Described soluble calcium salt is at least one in calcium chloride, nitrocalcite and lime acetate;
3), to step 2) filtrate that obtains carries out extraction treatment, and obtain extraction phase and extracting phase, extracting phase is pre-treatment water outlet; Extraction agent is one or more in the mixing solutions of tributyl phosphate and kerosene, benzene, toluene and hexanaphthene; Described extraction agent and step 2) volume ratio of filtrate that obtains is (0.5 ~ 2.5): 1.
2. pretreatment process as claimed in claim 1, is characterized in that, step 1) in sulphuric acid soln, the pH value of described acrylic ester wastewater is adjusted to 1.5 ~ 3.
3. pretreatment process as claimed in claim 2, is characterized in that, step 1) in sulphuric acid soln, the pH value of described acrylic ester wastewater is adjusted to 1.5 ~ 2.5.
4. the pretreatment process as described in any one of claims 1 to 3, is characterized in that, the dosage of described soluble salt is 0.2% ~ 0.3% of described acrylic ester wastewater quality.
5. pretreatment process as claimed in claim 4, is characterized in that, described extraction agent and step 2) volume ratio of filtrate that obtains is (1 ~ 1.5): 1.
6. pretreatment process as claimed in claim 5, is characterized in that, described extraction agent is at least one in the mixing solutions of tributyl phosphate and kerosene, Benzene and Toluene.
7. pretreatment process as claimed in claim 6, is characterized in that, also comprises and reclaims vinylformic acid in extraction phase.
8. pretreatment process as claimed in claim 1, it is characterized in that, in the mixing solutions of described tributyl phosphate and kerosene, the volume fraction of tributyl phosphate is 20% ~ 50%.
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| CN201510595519.3A CN105084608B (en) | 2015-09-17 | 2015-09-17 | A kind of preprocess method of acrylic ester wastewater biochemical treatment |
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| CN111559816A (en) * | 2019-02-13 | 2020-08-21 | 中国石油天然气股份有限公司 | Method for treating wastewater of methyl methacrylate device |
| CN115448834A (en) * | 2022-09-16 | 2022-12-09 | 卫星化学股份有限公司 | Method for refining acrylic acid aqueous solution |
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| CN115448834A (en) * | 2022-09-16 | 2022-12-09 | 卫星化学股份有限公司 | Method for refining acrylic acid aqueous solution |
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Denomination of invention: Pretreatment method of acrylate wastewater biochemical treatment Effective date of registration: 20191127 Granted publication date: 20170531 Pledgee: Beijing urban construction and development branch of China Construction Bank Co., Ltd Pledgor: POTEN ENVIRONMENT GROUP CO., LTD. Registration number: Y2019990000597 |