CN102092906B - Treatment and resource-utilizing technology of tert-butyl peroxy benzoate production wastewater - Google Patents
Treatment and resource-utilizing technology of tert-butyl peroxy benzoate production wastewater Download PDFInfo
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Abstract
The invention discloses a treatment and resource-utilizing technology of the production wastewater of tert-butyl peroxy benzoate (initiator is C). The technology is as follows: high concentration production wastewater is collected from the sewage outlet of a production device to perform stabilization treatment, and after the risk that the organic peroxide in wastewater is violently decomposed when heated is basically eliminated, the mixture of tertiary butanol and tert-butyl peroxide, sulfuric acid, benzoic acid and sodium chloride are recycled from wastewater. the mixture of tertiary butanol and tert-butyl peroxide, benzoic acid and sulfuric acid can be used repeatedly in production and sodium chloride is a by-product. After most of tertiary butanol and tert-butyl peroxide are removed and benzoic acid, sulfuric acid and sodium chloride are recycled, the wastewater performs hydrolysis-contact oxidation and C-Fe micro-electrolysis decoloring treatment and the main indexes of discharged water meet the requirements of the discharge standard of water pollutants for pharmaceutical industry chemical synthesis products category (GB21904-2008) on the water pollutants emission limits of new business.
Description
Technical field
The invention belongs to the technology for treating industrial waste water field, relate to a kind of organo-peroxide class production wastewater treatment and process for reclaiming, relate in particular to a kind of initiator peroxidized t-butyl perbenzoate production wastewater treatment and process for reclaiming.
Background technology
Peroxidized t-butyl perbenzoate (initiator C) is one of kind commonly used in the organic peroxide evocating agent.Be widely used in such as ethene, vinylbenzene, be used as initiator in the polymerization processes such as propylene, vinyl acetate between to for plastic, Phthalic acid, diallyl ester and iso-butylene.In the curable unsaturated polyester process, be widely used in as in the moulding processs such as SMC, BMC, DMC pultrusion, simultaneously, also can be with higher the using of some activity like the two component curing systems of compositions such as MEPK, BPO or TBPO.
The production process of peroxidized t-butyl perbenzoate (initiator C) is intermittently carried out, and the waste water quality water yield, organic concentration, potential of hydrogen, saltiness, BOD/CDO value etc. changed with industrial scale and time, and it is very big that peak-to-valley value differs.The peroxidized t-butyl perbenzoate thermally labile, accelerate decompsn is dissolved in the peroxidized t-butyl perbenzoate also decomposition rapidly at high temperature in the waste water easily.Production technique produces the high density spent acid, contains the synthesis mother liquid and the washing waste liquid of a large amount of Sodium Benzoates, sodium-chlor, sodium hydroxide.Pollutant levels are high in the waste water, complicated component, and containing has inhibiting phenylformic acid to biological degradation, and the B/C value is very low, can't biochemical treatment.This waste water directly enters the river can cause the water body severe contamination.
The raw materials for production of peroxidized t-butyl perbenzoate (initiator C) mainly contain the trimethyl carbinol, sulfuric acid, sodium hydroxide, ydrogen peroxide 50, Benzoyl chloride 99min. etc.Different steps producing produces waste water of different nature, mainly contains strongly acid wastewater, strong basicity waste water and product washing waste water etc.Strongly acid wastewater is that midbody---the production spent acid of tert-butyl peroxide mainly contains the trimethyl carbinol, tert-butyl peroxide, hydrogen peroxide, sulfuric acid, ditertiary butyl peroxide etc. in production.COD in the strongly acid wastewater
Cr=89878.40mg/L～109524.64mg/L, non-volatile solid (salt and silt) content 1.60%～1.97% (Wt).Strong basicity waste water is the synthetic waste liquid of initiator C, mainly contains the trimethyl carbinol, tert-butyl peroxide, peroxidized t-butyl perbenzoate, Sodium Benzoate, sodium hydroxide, sodium-chlor etc.COD in the strong basicity waste water
Cr=99924.80 mg/L～170955.8mg/L, non-volatile solid (salt, alkali and silt) content 15.6～16.7% (Wt).Contain the trimethyl carbinol, tert-butyl peroxide, peroxidized t-butyl perbenzoate, Sodium Benzoate, sodium-chlor etc. in the product washing waste water.In the product washing waste water, COD
Cr=45582.88～59878.40mg/L, non-volatile solid (salt, alkali and silt) content 3.80 ~ 16.00% (Wt).Because peroxidized t-butyl perbenzoate factory effluent high density, high salinity, high acidity or high basicity, thermally labile are the environmental protection difficult problems of a wastewater treatment aspect.
According to bibliographical information, at present for high saliferous, height contain acid, height contains alkali, the organo-peroxide waste water of difficult degradation generally adopts electrolysis, dilution is burned with dilution biochemical, methods such as desalination dilution biochemistry are handled.
A kind of exemplary process technology is organo-peroxide to be produced mixed collections such as waste liquid, product scrub raffinate, vent gas treatment waste lye, cooling tower sewer, equipment and ground wash-down water to acidulated pool; Add hydrochloric acid and transfer to PH between 2～4; Organism is separated out, carry out gravity settling then.The upper organic phase that sedimentation obtains is collected back adding diesel fuel dilution burns organo-peroxide concentration reduction back outward transport.Sedimentation gained lower floor sour water is sent into regional sewage work then and is diluted with 200 times of low salinity waters with the NaOH neutrality that neutralizes, and the saltiness that makes waste water utilizes three slot type oxidation ditches to carry out biochemical treatment less than 1% again.Biochemistry is suppressed when the trimethyl carbinol and sodium benzoate concentration are high.
The shortcoming of this treatment process is: the organo-peroxide waste strength is high, burns after the separating obtained organism of acidifying will add diesel fuel dilution, and resource does not reclaim, and waste is serious.Organic concentration is still than higher in the waste water after separating, and the component that suppresses mikrobe is many, has increased the processing load of regional sewage work.Zone sewage work will be provided with special equalizing tank to wastewater dilution, and is biochemical then.In addition, this treatment process only is fit to the very high alkaline waste water of concentration of treatment.The organic acid salt that solubleness is very big in alkaline waste water is converted into the lower organic acid of solubleness and separated, still very big to solubleness almost not effect of alcohols after acidifying, still contain large amount of organic in the waste water after the acidifying.
Summary of the invention
The present invention be directed to the deficiency that existing treatment technology exists, a kind of peroxidized t-butyl perbenzoate production wastewater treatment and process for reclaiming are provided.
Peroxidized t-butyl perbenzoate production wastewater treatment of the present invention and process for reclaiming; Be to get high density from the production equipment sewage draining exit to produce waste water; According to the accelerate decompsn temperature of contained organo-peroxide in the waste water, controlled temperature lets its slow decomposition at it below the accelerate decompsn temperature, and adds reductive agent reduction organo-peroxide; Eliminate the violent decomposition of dangerous of superoxide in the waste water, make waste water reach stable.Then to the waste water low-temperature distillation, utilize the trimethyl carbinol, tert-butyl peroxide to form the trimethyl carbinol and tert-butyl peroxide in the characteristic Separation and Recovery waste water of minimum boiling point azeotrope with water.Strongly acid wastewater goes out lower concentration acid waste water through the normal pressure fractionation by distillation, and the spent acid after concentrating reclaims the vitriol oil through underpressure distillation; The pH value of adjustment strong basicity waste water therefrom reclaims phenylformic acid; Strong basicity waste water and washing waste water Separation and Recovery chlorination sodium in the distillation concentration process.Isolated low concentration wastewater is handled through neutralization, acidication-catalytic oxidation, again through the little electrolysis process of C-Fe.The draining leading indicator reach " chemosynthesis class pharmaceutical industry pollution discharge standard " (GB21904-2008) in to the requirement of newly-built enterprise water pollutant emission limit.
Concrete technology is following:
(1) peroxidized t-butyl perbenzoate is produced the processing of spent acid
Collect peroxidized t-butyl perbenzoate from the production equipment sewage draining exit and produce spent acid, add 0.8 ~ 1.2 gram S-WAT in every liter of waste water, slowly be heated to 50 ~ 60 ℃, stir air distillation after 1.5 ~ 2.0 hours.Layering behind distillate condensation, the cool to room temperature, upper strata are organic phase, and lower floor is a water.Reclaim the organic phase on upper strata, obtain the mixture of the trimethyl carbinol and tert-butyl peroxide, utilize the heterogeneous separation technique dehydration to purify, can reuse.Aqueous-phase reflux.When treating that distillate does not have layering at normal temperatures, continue fractionation by distillation and go out lower concentration acid waste water, after lower concentration acid waste water is neutralized to PH=7～8, through hydrolysis-catalytic oxidation, qualified discharge after the little electrolysis process of C-Fe is handled again.Concentrating waste acid after the distillation reclaims the vitriol oil through the water-circulating pump underpressure distillation, but reclaims the distillation residue landfill disposal that the vitriol oil produces.
(2) peroxidized t-butyl perbenzoate strong basicity production wastewater treatment
Get the strong basicity waste water that synthesizes peroxidized t-butyl perbenzoate from the production equipment sewage draining exit, add 0.8 ~ 1.2 gram sodium sulphite in every liter of waste water, be heated to 50 ~ 60 ℃, stirred 1.5 ~ 2 hours.At room temperature be neutralized to PH＜5 after-filtration and isolate, reclaim phenylformic acid with hydrochloric acid.Filtrating is through the water-circulating pump underpressure distillation, and fractionation obtains the trimethyl carbinol and tert-butyl peroxide mixture, the trimethyl carbinol of recovery and the mixture of tert-butyl peroxide.Mother liquor continues fractionation by distillation and goes out the slightly acidic low concentration wastewater, after the lower concentration acid waste water that separation obtains is neutralized to neutrality, and qualified discharge after hydrolysis-catalytic oxidation, the little electrolysis process of C-Fe are handled; Crystallization goes out sodium-chlor in the mother liquor distillation concentration process, and filtering purifies obtains sub product sodium-chlor.
Acidifying separates the phenylformic acid obtain and use dissolution of sodium hydroxide, filters out body refuse, again with hcl acidifying to PH 5, filter out phenylformic acid, dry the phenylformic acid product, filtrate and return Distallation systm.
The trimethyl carbinol that fractionation obtains and tert-butyl peroxide mixture utilize the heterogeneous separation technique dehydration to purify, and can be recycled and reused for production.
(3) processing of peroxidized t-butyl perbenzoate product washing waste water
Get the washing waste water of synthetic peroxidized t-butyl perbenzoate product from the production equipment sewage draining exit.To wash waste water and be preheating to 50 ~ 60 ℃, slowly add 0.8 ~ 1.2 gram S-WAT in every liter of waste water, stir 1.5 ~ 2 hours.The adjustment potential of hydrogen use the water-circulating pump underpressure distillation to PH ﹥ 7, isolates low concentration wastewater, be neutralized to neutrality after, qualified discharge after the little electrolysis process processing of hydrolysis-catalytic oxidation, C-Fe.Crystallization goes out sodium-chlor, filtered and recycled sodium-chlor in the distillation concentration process.
The sodium-chlor that reclaims is used alkaline water drip washing, obtains refining sodium-chlor, content with a small amount of tap water drip washing again>98.%, reach industrial purified salt quality standard.The phenylformic acid that ring waste acidifying after-filtration obtains, filtrating are incorporated next time into and are separated.
The present invention compared with prior art has the following advantages:
1, the present invention gets high density from the production equipment sewage draining exit and produces waste water; Organic Chemicals, sodium-chlor and sulfuric acid in elder generation's Separation and Recovery waste water; Carry out biochemical treatment again, make processed waste water reach " chemosynthesis class pharmaceutical industry pollution discharge standard " (GB21904-2008) in to the requirement of newly-built enterprise water pollutant emission limit.
2, a large amount of Chemical Manufacture material purities that from waste water, reclaim are high, and quality is good, reaches the repeated use requirement, has realized the recycling of pollutent in the waste water, meets the demand for development of recycling economy, energy-saving and emission-reduction.
3, the present invention combines closely and produces actually, reasonable in design, and technological line is advanced, operates easylier, and treating processes does not produce secondary pollution.
4, burn, dilute biochemical technology relatively with electrolysis, the dilution of domestic and foreign current, in the biochemical treatment that has realized used water difficult to degradate, reclaimed a large amount of Chemical Manufacture raw materials, practiced thrift processing costs, protected resource and environment effectively.
Embodiment
Through specific examples the processing and the recycling technology of peroxidized t-butyl perbenzoate of the present invention (initiator C) factory effluent are carried out detailed explanation below.
(1) peroxidized t-butyl perbenzoate is produced the processing of spent acid
Collect the spent acid that 11.5 liters of peroxidized t-butyl perbenzoates are produced from the production equipment sewage draining exit.Sulfur acid＞40% wherein, COD
Cr=83460.96mg/L.
Add 12 gram S-WATs (adding 1 gram S-WAT in every liter of waste water) in the spent acid, slowly be heated to 50 ~ 60 ℃, stir air distillation after 1.5 ~ 2.0 hours, layering behind distillate condensation, the cool to room temperature, the upper strata is an organic phase, lower floor is a water.Reclaim the organic phase on upper strata, utilize the mixture 900ml that obtains the trimethyl carbinol and tert-butyl peroxide behind the heterogeneous separation technique distillation dehydration,, can be recycled and reused for production through gas chromatographic analysis total content 99.84%.Lower floor's aqueous-phase reflux.When treating that distillate does not have layering at normal temperatures, continue fractionation by distillation and go out lower concentration acid waste water, after lower concentration acid waste water is neutralized to PH=7～8, through hydrolysis-catalytic oxidation, qualified discharge after the little electrolysis process processing of C-Fe in 30 minutes again; Concentrating waste acid after the distillation reclaims vitriol oil 6500ml through the water-circulating pump underpressure distillation, can be recycled and reused for production.But reclaim the distillation residue landfill disposal that produces behind the vitriol oil.
(2) peroxidized t-butyl perbenzoate strong basicity production wastewater treatment
Get the strong basicity waste water of 18 liters of synthetic peroxidized t-butyl perbenzoates from the production equipment sewage draining exit.Wherein, COD
Cr=99924.64mg/L; Contain NaOH 13.6g/L through titration, contain non-volatile solid 16.70%.
Add 18 gram sodium sulphite (adding 1 gram sodium sulphite in every liter of waste water) in the waste water, be heated to 50 ~ 60 ℃, stirred 1.5 ~ 2 hours.At room temperature be neutralized to PH＜5 after-filtration and isolate phenylformic acid, recycle with hydrochloric acid.Filtrating (COD
Cr=41035.68mg/L) through the water-circulating pump underpressure distillation, fractionation obtains the trimethyl carbinol and tert-butyl peroxide mixture 1000ml.Mother liquor continues fractionation by distillation and goes out slightly acidic low concentration wastewater (COD
Cr=4559.2mg/L, CODcr clearance 99.44%).After the lower concentration acid waste water that separation obtains is neutralized to about PH=7, qualified discharge after hydrolysis-catalytic oxidation, the little electrolysis process of C-Fe are handled.
Crystallization goes out sodium-chlor in the mother liquor distillation concentration process, filters out sodium-chlor and uses alkaline water drip washing earlier, uses tap water drip washing to neutral again, obtains purified sodium-chlor 4.75kg after the oven dry.The phenylformic acid that ring waste acidifying after-filtration obtains, filtrating are incorporated next time into and are separated.
Acidifying separates the phenylformic acid obtain and uses dissolution of sodium hydroxide, filters out body refuse, again with hcl acidifying to PH 5, filter out phenylformic acid, dry the phenylformic acid product 0.5kg of purity 99.76%.But the body refuse burning disposal that filters out.
The trimethyl carbinol that reclaims and tert-butyl peroxide mixture utilize the heterogeneous separation technique dehydration to purify, and total concn reaches 99.84%, can be recycled and reused for production.
(3) processing of peroxidized t-butyl perbenzoate product washing waste water
Get the washing waste water of 20 liters of synthetic peroxidized t-butyl perbenzoate products from the production equipment sewage draining exit.CODcr=59878.40mg/L in the former water; PH=5; Contain non-volatile solid 16.00%.
Waste water is preheating to 50 ~ 60 ℃,, stirred 1.5 hours to wherein slowly adding 20 gram S-WATs (adding 1 gram S-WAT in every liter of waste water).The adjustment potential of hydrogen is used the water-circulating pump underpressure distillation to PH ﹥ 7, isolates low concentration wastewater (COD
Cr=230.78mg/L～740.16mg/L, the CODcr clearance is 99.61%～98.76%), be neutralized to about PH=7 after, qualified discharge after hydrolysis-catalytic oxidation, the little electrolysis process of C-Fe are handled.
Crystallization goes out sodium-chlor in the distillation concentration process, filtered and recycled sodium-chlor, and filtrating is returned underpressure distillation.The sodium-chlor that reclaims is used alkaline water drip washing, obtains the refining sodium-chlor of 4.5kg, content with a small amount of tap water drip washing, oven dry again>98.%.The phenylformic acid that ring waste acidifying after-filtration obtains, filtrating are incorporated next time into and are separated.
Be the detected result that reclaims the raw materials for production quality and handle the back discharge water below:
1. reclaim the quality examination result of the trimethyl carbinol-tert-butyl peroxide
The raw materials for production that from spent acid and strong basicity waste water, reclaim---the trimethyl carbinol and tert-butyl peroxide mixture are through the gas chromatographic analysis total content: 99.84%.
2. reclaim(ed) sulfuric acid quality examination result
| Analytical element | Analytical results % (Wt) | Analytical element | Analytical results % (Wt) |
| H 2SO 4 | 97.60 | Hg | 0.000004 |
| Ash content | 0.009 | Pb | 0.00002 |
| Fe | 0.00005 | Transparency | ＞50 mm |
| As | 0.000003 | Colourity | ＜2.0ml |
3. reclaim the quality examination result of sodium-chlor
| Analysis project | Analytical results % (Wt) |
| NaCl | 98.24 |
| Ca 2＋ | 0.01 |
| Mg 2+ | 0.01 |
| SO 4 2＋ | 0.10 |
| Moisture | 0.04 |
| Water-insoluble | 0.29 |
4. reclaim benzoic quality examination result:
Outward appearance: flakey or needle-like colourless crystallization are soft;
Fusing point: 121.0～123.5 ℃;
Content: 99.76%.
2. draining WQM result after the biochemical treatment:
①?pH?：6-9；
2. colourity
< 5;
3. COD (COD
Cr)<100mgL;
4. five-day BOD (BOD
5)<25mgL;
5. suspended substance does not detect;
6. volatile phenol does not detect.
Claims (4)
1. peroxidized t-butyl perbenzoate production wastewater treatment and process for reclaiming is characterized in that: comprise following process step:
(1) peroxidized t-butyl perbenzoate is produced the processing of spent acid
Collect peroxidized t-butyl perbenzoate from the production equipment sewage draining exit and produce spent acid, add 0.8 ~ 1.2 gram S-WAT in every liter of spent acid, slowly be heated to 50 ~ 60 ℃; Stir air distillation after 1.5 ~ 2.0 hours; Layering behind distillate condensation, the cool to room temperature, upper strata are organic phase, and lower floor is a water; Reclaim the organic phase on upper strata, obtain the trimethyl carbinol and tert-butyl peroxide mixture; Aqueous-phase reflux; When treating that distillate does not have layering at normal temperatures, continue fractionation by distillation and go out lower concentration acid waste water, after lower concentration acid waste water is neutralized to pH=7～8, through hydrolysis-catalytic oxidation, qualified discharge after the little electrolysis process of C-Fe is handled again; Concentrating waste acid after the distillation reclaims the vitriol oil through the water-circulating pump underpressure distillation;
(2) peroxidized t-butyl perbenzoate strong basicity production wastewater treatment
Get the strong basicity waste water that synthesizes peroxidized t-butyl perbenzoate from the production equipment sewage draining exit, add 0.8 ~ 1.2 gram sodium sulphite in every liter of waste water, be heated to 50 ~ 60 ℃, stirred 1.5 ~ 2 hours, at room temperature be neutralized to pH＜5 after-filtration and separate, reclaim phenylformic acid with hydrochloric acid; Filtrating is through the water-circulating pump underpressure distillation, and the trimethyl carbinol and tert-butyl peroxide mixture are reclaimed in fractionation; Mother liquor continues fractionation by distillation and goes out the slightly acidic low concentration wastewater, separates the lower concentration acid waste water that obtains and is neutralized to neutrality, qualified discharge after hydrolysis-catalytic oxidation, the little electrolysis process of C-Fe are handled; Crystallization goes out sodium-chlor in the mother liquor distillation concentration process, and filtering purifies obtains sub product sodium-chlor;
(3) processing of peroxidized t-butyl perbenzoate product washing waste water
Get the washing waste water that synthesizes the peroxidized t-butyl perbenzoate product from the production equipment sewage draining exit, waste water is preheating to 50 ~ 60 ℃, add 0.8 ~ 1.2 gram S-WAT in every liter of waste water, stirred 1.5 ~ 2 hours; The adjustment potential of hydrogen is used the water-circulating pump underpressure distillation to pH ﹥ 7, isolates low concentration wastewater, is neutralized to neutrality, qualified discharge after hydrolysis-catalytic oxidation, the little electrolysis process of C-Fe are handled; Crystallization goes out sodium-chlor, filtered and recycled sodium-chlor in the distillation concentration process.
2. peroxidized t-butyl perbenzoate production wastewater treatment and process for reclaiming according to claim 1, it is characterized in that: the trimethyl carbinol that reclaim step (1), (2) and the mixture of tert-butyl peroxide utilize heterogeneous separation technique dehydration purification.
3. peroxidized t-butyl perbenzoate production wastewater treatment and process for reclaiming according to claim 1; It is characterized in that: step (2) is neutralized to the phenylformic acid that pH＜separation of 5 after-filtration obtains with hydrochloric acid and uses alkali dissolution; Filter out body refuse, be acidified to again pH 5, and filter, dry the phenylformic acid product.
4. peroxidized t-butyl perbenzoate production wastewater treatment and process for reclaiming according to claim 1; It is characterized in that: the sodium-chlor that reclaim step (2), (3) is used earlier alkaline water drip washing; Use tap water drip washing to neutral again, obtain purified sodium-chlor product after the oven dry.
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| CN102965506B (en) * | 2012-12-14 | 2015-07-22 | 葛新芳 | Method for removing aluminum from rare earth solution by benzoate precipitation method |
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| CN108610273B (en) * | 2018-06-13 | 2019-11-01 | 江苏强盛功能化学股份有限公司 | A kind of method of purification of peroxidized t-butyl perbenzoate |
| CN109020786B (en) * | 2018-09-21 | 2022-03-25 | 常熟市滨江化工有限公司 | Resourceful treatment method of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane mother liquor |
| BR112021024870A2 (en) * | 2019-06-12 | 2022-01-18 | Nouryon Chemicals Int Bv | Method for isolating carboxylic acid from an aqueous side stream of an organic peroxide production process |
| JP7336541B2 (en) | 2019-06-12 | 2023-08-31 | ヌーリオン ケミカルズ インターナショナル ベスローテン フェノーツハップ | Process for producing diacyl peroxide |
| US11976034B2 (en) | 2019-06-12 | 2024-05-07 | Nouryon Chemicals International B.V. | Process for the production of diacyl peroxides |
| CN110330189B (en) * | 2019-07-25 | 2022-03-08 | 四川恒泰环境技术有限责任公司 | Treatment method of wastewater containing benzoic acid |
| CN113105049A (en) * | 2021-03-24 | 2021-07-13 | 广东丽臣奥威实业有限公司 | Treatment method of sewage containing high-foam surfactant |
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