CN110482756A - A kind of method of epoxychloropropane utilization of wastewater resource - Google Patents
A kind of method of epoxychloropropane utilization of wastewater resource Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/10—Treatment of water, waste water, or sewage by heating by distillation or evaporation by direct contact with a particulate solid or with a fluid, as a heat transfer medium
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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Abstract
The present invention provides a kind of epoxychloropropane waste water reclaiming processing scheme, pass through stripping, grease layering, filtering, reverse osmosis membrane apparatus concentration, resin adsorption, the technique of resin regeneration, moisture and organic matter can be efficiently separated, realize epoxychloropropane in waste water, glycerine monochlorohydrin recycling, standard water discharge discharge, has a extensive future.
Description
Technical field
The invention belongs to waste water treatment process technical fields, and in particular to organic in a kind of recycling epoxychloropropane waste water
Object, the method for realizing waste water reclaiming.
Background technique
Epoxychloropropane is a kind of volatile, unstable colourless oil liquid, water is slightly soluble in, mainly for the manufacture of epoxy
Resin and epoxy group and phenoxy resin primary raw material.Epichlorohydrin production process is mainly chlorohydrination and glycerol at present
Method.Chlorohydrination wastewater flow rate is big, and environmental pollution is serious, belongs to restricted technique.Glycerol method is limited by the supply of glycerol, continues growing production
The difficulty of energy is big, is unable to satisfy growing demand.In this context, use chloropropene for raw material, hydrogen peroxide is oxidant,
Catalysis epoxidation prepares epoxychloropropane, and due to atom utilization height, wastewater flow rate is few, and process route cleaning becomes researcher and closes
Heat injection point.It is the reaction system of catalyst due to its special reaction phase transfer characteristic using heteropoly acid, catalyst easily recycles and steady
It is qualitative good, there is preferable prospects for commercial application.
Using heteropoly acid catalysis system epoxy chloropropane by hydrogen peroxide method, reaction terminates that 0.8-1t waste water/t ring can be generated
Oxygen chloropropane, waste water not saliferous, 30000~80000ppm of COD, main 0.05~1.0% epoxychloropropane of organic matter, 1.0~
5.0% glycerine monochlorohydrin, this effluent part COD high, organic concentration is high, and direct biochemical treatment can cause to rush to biochemical strain
It hits, needs to pre-process and the amount of increasing water dilutes, increase processing cost and wastewater flow rate, cause the wasting of resources, reduce peroxide passivation
The economy of epoxychloropropane.
Patent CN105271597B discloses a kind of epoxychloropropane producing wastewater treatment, passes through light electrolysis, depth
The kinds of processes such as oxidation, flocculation sedimentation, absorption retardance, UF membrane are directed to epoxychloropropane waste water by specific combination
Property online processing, COD numerical value can be significantly reduced, effect is obvious, but process is tedious, and processing cost is high.
A kind of processing unit of the epoxychloropropane production waste water based on membrane separation technique of patent CN206705802U, passes through
Epoxychloropropane waste water is adsorbed, film filtration treatment, can preferably remove the organic and inorganic impurity in waste water, is handled
Waste water afterwards passes through the higher salt of the available purity of concentration and recovery, but does not refer to that organic resourcesization utilize in waste water.
Patent CN105621764B discloses a kind for the treatment of process of epoxychloropropane production waste water, by wet oxidation,
Photocatalysis oxidation technique realizes the resource utilization of salt in waste water.But the technology can not recycle useless Organic substance in water, and
Wet-type oxidation technology high temperature and pressure, equipment material require height, and investment is big.
Summary of the invention
In order to overcome the shortcomings of in the prior art, the present invention is intended to provide a kind of epoxychloropropane waste water reclaiming processing side
Case can efficiently separate moisture and organic matter by a series for the treatment of process, realize in waste water epoxychloropropane, a chlorine the third two
Alcohol recycling, standard water discharge discharge, has a extensive future.
To achieve the goals above, the present invention provides a kind of method of epoxychloropropane utilization of wastewater resource, including with
Lower step:
The first step, epoxychloropropane waste water enter stripper after preheating, and stripping discharging enters oil-water decanter, water layer
Stripping tower reactor, oil reservoir recycling are returned to, stripping tower reactor water enters next process；
Second step, the cooling of stripping vessel water removes mechanical admixture by accurate filter, then is delivered to by force (forcing) pump reverse osmosis
Film device obtains production water by reverse osmosis membrane and enters next process, obtain one by reverse osmosis membrane under certain pressure effect
Determine the dope of concentration, dope is used to prepare epoxychloropropane after enrichment facility continues concentrate；
Third step, reverse osmosis produced water are pumped into the adsorption tower of potting resin with circulating pump, using upper entering and lower leaving mode, adsorption tower
Standard water discharge discharge.
The hot water of 4th step, the resin certain temperature of adsorption saturation parses regeneration, obtains a certain concentration desorbed solution, returns
Second step filtering, reverse osmosis process.
Based on the above technical solution, stripping process described in the first step, stripping tower reactor kettle temperature control is 90~110
DEG C, strip the number of plates 5~20.
Based on the above technical solution, reverse osmosis process described in second step, stripping tower reactor water are cooled to 25~35
℃。
Based on the above technical solution, reverse osmosis process described in second step, pressure are 3~5MPa；
Based on the above technical solution, reverse osmosis process described in second step produces glycerine monochlorohydrin concentration in water
0.05~0.2%；
Based on the above technical solution, reverse osmosis process described in second step, glycerine monochlorohydrin concentration 15 in dope
~30%；
Based on the above technical solution, adsorption process described in third step, adsorption tower flow of inlet water be 0.5~
2.0BV/h；
Based on the above technical solution, adsorption process described in third step selects resin to provide for Xi'an indigo plant dawn big
Hole resin；
Based on the above technical solution, adsorption process described in third step, adsorption tower are discharged glycerine monochlorohydrin concentration
≤ 0.02%, COD≤300ppm；
Based on the above technical solution, the parsing of saturated resin described in the 4th step regenerative process, hot water temperature 60~
80℃；
Based on the above technical solution, saturated resin described in the 4th step parses regenerative process, a chlorine in desorbed solution
PG concentration 1.0~10%.
Compared with prior art, the present invention has the following advantages:
(1) water and organic matter in epoxychloropropane waste water are efficiently separated, utilization of wastewater resource is solved and qualified discharge is asked
Topic；
(2) epoxychloropropane is dissolved in stripping recycling waste water, improves the yield of target product；
(3) reverse osmosis membrane concentrate glycerine monochlorohydrin avoids direct concentration protocol from consuming a large amount of steam, at low cost；
(4) using a small amount of glycerine monochlorohydrin in suction type recycling reverse osmosis produced water, glycerine monochlorohydrin receipts are further increased
Rate reduces water outlet COD content, it is ensured that qualified discharge；
(5) process flow is easy, and operating condition is mild, and treatment effect is reliable and stable, is easy to industrializing implementation.
Detailed description of the invention
The flow diagram of Fig. 1 epoxychloropropane utilization of wastewater resource of the present invention.
Specific embodiment
Company's workshop epoxychloropropane waste water, COD 55630ppm, pH about 3, epoxychloropropane 0.8%, a chlorine third
Glycol 3.0%.
Embodiment 1
(1) it strips
Epoxychloropropane waste water enters stripper after preheating, in 95-105 DEG C of stripper operating temperature, tiny structure-
0.025Mpa, under conditions of 10 pieces of theoretical cam curve, stripping discharging enters oil-water decanter, oil reservoir recycling, and water layer returns to stripping
Tower reactor strips tower reactor kettle water COD 42710ppm, epoxychloropropane is not under the conditions of stripping tower top quantity of distillate is tower amount 7.0%
Detection, glycerine monochlorohydrin 3.1%.
(2) reverse osmosis concentration
Stripping tower reactor water is cooled to 25~35 DEG C, is crossed by accurate filter and filters out mechanical admixture, passes through pressurization after filtering
Pump is delivered to reverse osmosis membrane enrichment facility, pressure 4.0MPa, and reverse osmosis membrane is concentrated 7.2 times, and reverse osmosis membrane produces water COD
2780ppm, glycerine monochlorohydrin 0.15%, glycerine monochlorohydrin content 21.4% in reverse osmosis membrane dope pass through enrichment facility negative pressure
Distillation is by glycerine monochlorohydrin concentration concentrate in dope to 50% to prepare epoxychloropropane up.
(3) resin adsorption
The macroreticular resin that absorption is provided using Xi'an indigo plant dawn, adsorption tower fill 3m3Resin, reverse osmosis produced water as adsorption tower into
Water passes through resin adsorption tower, and flow of inlet water 1BV/h, water outlet is colorless and transparent, and COD 95ppm, glycerine monochlorohydrin is not examined
Out, pH=7.0 meets emission request.Inflow 60BV or so resin saturation, is regenerated.
(4) resin regeneration
Regeneration uses 60~80 DEG C of hot water, passes through resin adsorption tower, hot water flow 1BV/h, out desorbed solution 2BV
Left and right resin regeneration is finished, and is obtained desorbed solution and is gone filtering, reverse osmosis concentrated compression apparatus.Glycerine monochlorohydrin overall recovery 99.90%.
Embodiment 2
Reverse osmosis concentration pressure process is reduced on that basis of example 1 to 3.0MPa, obtains producing water COD 1765ppm, one
Propylene glycol of chlorine 0.09%, glycerine monochlorohydrin 15.0% in reverse osmosis membrane dope are concentrated into 50% further to prepare epoxy up
Chloropropane.Reverse osmosis produced water enters resin adsorption tower with 1BV/h speed, is discharged COD 80ppm, and glycerine monochlorohydrin is not detected, pH
=7.0, meet emission request.100BV or so resin of intaking is saturated, and is regenerated with 60~80 DEG C of hot water, glycerine monochlorohydrin is total
Yield 99.95%.
Embodiment 3
Reverse osmosis concentration pressure process is improved on the basis of example 1 to 5.0MPa, obtains producing water COD 3290ppm, a chlorine
Propylene glycol 0.20%, glycerine monochlorohydrin 30.0% in reverse osmosis membrane dope are concentrated into 50% further to prepare epoxy chlorine up
Propane.Reverse osmosis produced water enters resin adsorption tower with 1BV/h speed, is discharged COD 95ppm, and glycerine monochlorohydrin is not detected, pH=
7.0, meet emission request.Water inlet is regenerated, glycerine monochlorohydrin is total up to 45BV or so resin saturation with 60~80 DEG C of hot water
Yield 99.93%.
Embodiment 4
On the basis of example 1, resin adsorption water intake velocity is adjusted, reverse osmosis produced water enters resin with 0.5BV/h speed and inhales
Attached tower is discharged COD 83ppm, and glycerine monochlorohydrin is not detected, pH=7.0, meets qualified discharge requirement, water inlet 60BV or so resin
Saturation is regenerated, glycerine monochlorohydrin total recovery 99.96% with 60~80 DEG C of hot water.
Embodiment 5
On the basis of example 1, resin adsorption water intake velocity is adjusted, reverse osmosis produced water enters resin with 2.0BV/h speed and inhales
Attached tower is discharged COD 235ppm, glycerine monochlorohydrin 0.01%, pH=6.9, meets qualified discharge requirement, water inlet 64BV or so tree
Rouge saturation, is regenerated, glycerine monochlorohydrin total recovery 99.77% with 60~80 DEG C of hot water.
Claims (10)
1. a kind of method of epoxychloropropane utilization of wastewater resource, comprising the following steps:
The first step, epoxychloropropane waste water enter stripper after preheating, and stripping discharging enters oil-water decanter, and water layer returns
Tower reactor, oil reservoir recycling are stripped, stripping tower reactor water enters next process；
Second step, the cooling of stripping vessel water removes mechanical admixture by accurate filter, then is delivered to reverse osmosis membrane dress by force (forcing) pump
It sets, under certain pressure effect, production water is obtained by reverse osmosis membrane and enters next process, under certain pressure effect, is passed through
Reverse osmosis membrane obtains production water and enters next process, obtains certain density dope by reverse osmosis membrane, dope is by concentration dress
It sets and is used to prepare epoxychloropropane after continuing concentrate；
Third step, reverse osmosis produced water are pumped into the adsorption tower of potting resin with circulating pump, using upper entering and lower leaving mode, adsorption tower water outlet
Qualified discharge；
The hot water of 4th step, the resin certain temperature of adsorption saturation parses regeneration, obtains a certain concentration desorbed solution, returns to second
Step filtering, reverse osmosis process.
2. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that described
Stripping process described in one step, stripping tower reactor kettle temperature control is 90~110 DEG C, strips the number of plates 5~20.
3. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that described
Reverse osmosis process described in two steps, stripping tower reactor water are cooled to 25~35 DEG C.
4. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that described
Reverse osmosis process described in two steps, pressure are 3~5Mpa.
5. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that described
Reverse osmosis process described in two steps produces glycerine monochlorohydrin concentration 0.05~0.2% in water.
6. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that second step
Described in reverse osmosis process, glycerine monochlorohydrin concentration 15~30% in dope.
7. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that described
Adsorption process in three steps, adsorption tower flow of inlet water are 0.5~2.0BV/h.
8. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that described
Adsorption process in three steps, adsorption tower are discharged glycerine monochlorohydrin concentration≤0.02%, COD≤300ppm.
9. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that described
Saturated resin parsing regenerative process in four steps, 60~80 DEG C of hot water temperature.
10. a kind of method of epoxychloropropane utilization of wastewater resource according to claim 1, which is characterized in that described
Saturated resin parses regenerative process, glycerine monochlorohydrin concentration 1.0~10% in desorbed solution in 4th step.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253007A (en) * | 2020-02-24 | 2020-06-09 | 江苏扬农化工集团有限公司 | Method for treating epichlorohydrin wastewater |
| CN112076627A (en) * | 2020-09-15 | 2020-12-15 | 江苏扬农化工集团有限公司 | Method for applying reverse osmosis membrane and permeable membrane to separation of epoxy chloropropane |
| CN113880345A (en) * | 2021-11-06 | 2022-01-04 | 普林斯(安庆)医药科技有限公司 | Recovery treatment process of organic chloride |
| CN115043539A (en) * | 2022-04-20 | 2022-09-13 | 江苏瑞祥化工有限公司 | Treatment method of wastewater in epoxy resin production |
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| CN113880345B (en) * | 2021-11-06 | 2022-12-13 | 普林斯(安庆)医药科技有限公司 | Recovery treatment process of organic chloride |
| CN115043539A (en) * | 2022-04-20 | 2022-09-13 | 江苏瑞祥化工有限公司 | Treatment method of wastewater in epoxy resin production |
| CN115043539B (en) * | 2022-04-20 | 2024-02-09 | 江苏瑞祥化工有限公司 | Treatment method of wastewater in epoxy resin production |
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