CN104291523A - Method for recovering sodium chloride and glycerin from glycerin-containing high-salinity organic wastewater - Google Patents
Method for recovering sodium chloride and glycerin from glycerin-containing high-salinity organic wastewater 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
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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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
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F2001/5218—Crystallization
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
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Abstract
The invention discloses a method for recovering sodium chloride and glycerin in glycerin-containing high-salinity organic wastewater, which relates to the treatment of organic wastewater. The method comprises the following steps that: 1) the organic wastewater passes through macroporous resin, so that glycerin molecules in the wastewater are adsorbed, and macroporous resin with the glycerin molecules and sodium chloride-containing effluent are obtained; 2) the sodium chloride-containing effluent obtained in the step 1) is evaporated and concentrated in an evaporator, thus obtaining a sodium chloride concentrated solution; 3) the sodium chloride concentrated solution obtained in the step 2) is crystallized, thus obtaining solid sodium chloride and mother liquor left after crystallization and filtration; 4) after being diluted and biochemically treated, the mother liquor is discharged; 5) the macroporous resin treated in the step 1) is washed by using a desorption agent so as to elute the glycerin adsorbed on the macroporous resin to obtain glycerin-containing eluant and the macroporous resin subjected to eluting is put into the step 1) for cyclical utilization; 6) the glycerin-containing eluant obtained after desorption in the step 5) is distilled so as to obtain the desorption agent and crude glycerin, and the desorption agent is put into the step 5) for cyclical utilization; and 7) the crude glycerin obtained in the step 6) is fractionated, thus obtain a finished glycerin product and distillation residue liquid.
Description
Technical field
The present invention relates to treatment of Organic Wastewater, particularly the high salt of one is containing sodium-chlor and glycerine recovery method in glycerine organic waste water.
Background technology
Along with industrial expansion, the quantity discharged of organic waste water is increasing, processes organic waste water, make its qualified discharge or recycling utilization significant.In the industrial production such as soapmaking industry, epoxy chloropropane production, production of biodiesel, glycerol production, can produce the organic waste water of a large amount of high salt also containing finite concentration glycerine, its sodium chloride concentration is about 5% ~ 25%, glycerol content about 3% ~ 15%, COD
crbe about 20000 ~ 350000mg/L.The characteristic of high salt makes it be difficult to adopt bioprocess technology to process, and is also difficult to adopt membrane sepn, electrodialysis separation is separated with capacitive adsorption, and may causes heavy corrosion to treatment facility.At present, high salt containing Glycerol Wastewater treated side degree of facing danger or disaster greatly, high in cost of production problem.
Glycerine as important industrial chemicals, in the equal tool of industry utility values widely such as organic chemical industry, Polymer Synthesizing, household chemicals, textiles, coating, leather, tobacco, food and medicines.For many years, China is always at a large amount of import glycerine, and glycerol market remains very fast development.In addition, sodium-chlor, as the important raw materials for production of the industry such as chlor-alkali, also has very high using value.Therefore, how effectively processing containing Glycerol Wastewater high salt, make it reach emission standard to alleviate the pollution to environment, the recycling simultaneously realizing glycerine and sodium chloride has great value.
Chinese patent CN85105641 discloses a kind of method reclaiming glycerine from salt solution.This treatment process comprises evaporation removing moisture, and at least precipitates the salinity of about 85%; Liquid product is separated from deposited salt; Dilution liquid product makes its viscosity lower than 10 centipoises; Electrodialysis obtains dilution water flow further; Fractionation is to reclaim glycerine.This technique can realize sodium-chlor in waste water and sweet oil recovery, but facility investment is large, and complex manufacturing, cost is high, operation energy consumption is large, and equipment corrosion is serious.
It take glycerine as treatment process and the device of the waste water of raw material production epoxy chloropropane that Chinese patent CN101531442 discloses a kind of.This treatment process, according to the difference of sodium-chlor, water and glycerol molecule diameter, adopts the sorbing material similar to glycerol molecule diameter to adsorb glycerine.The advantage of this treatment process is: using the change salt solution of the sodium chloride-containing waste water after process as chlorine industry, thus realizes recycling, and the rinse water containing lower concentration glycerine can safety dumping after Biochemical method.But this technique the unrealized recycling to byproduct glycerine, cause waste.
It take glycerine as treatment process and the device of the brine waste of raw material production epoxy chloropropane that Chinese patent CN102153230A discloses a kind of.Brine waste and other are polluted lower waste water and mix by this treatment process, make saltiness lower than 5%, add nitrogen, phosphorus nutrition thing; Waste water is introduced moving-bed membrane bioreactor, utilize active sludge to further process; Waste water is introduced ozone reaction unit and carry out ozone Oxidation Treatment; Discharge.The advantage of this treatment process is: treating processes is simple, stable and cost is low, and effluent quality can be ensured.But this technique must utilize the lower waste water of saltiness to be in harmonious proportion, waste is caused to the byproduct such as sodium-chlor and glycerine a large amount of in waste water.
Chinese patent CN103073086A discloses a kind of glycerinated method in borated resin absorption waste water.The principle that this treatment process can react with glycerine based on boric acid is set up.By boric acid process large pore anion resin, form borate type ion exchange resin; Resin is inserted in glycerinated wastewater treatment equipment and adsorbs; When glycerol content reaches set amount in the water outlet of pending device, take out resin and by acid-alkali treatment wash-out boric acid glycerin complex compound, then borate type ion exchange resin recycled.This technique is 30% ~ 50% to the clearance of glycerine in waste water, can realize the recycling to glycerine, but along with the rising of sodium chloride concentration, the adsorptive capacity of resin declines, and this method is inapplicable containing Glycerol Wastewater to high salt.
Above method all provides sweet oil treatment process in brine waste, but not yet has a kind of method to provide high salt to contain the efficient recovery method of salinity and glycerine in Glycerol Wastewater.For a long time, China's contour salt of most epoxy resin production waste-waters is in discharge beyond standards state all the time containing Glycerol Wastewater, and high density sodium-chlor wherein and glycerine are not all recycled utilization, not only contaminate environment, and cause significant wastage to resource.
Summary of the invention
The object of the invention is to for the deficiency of existing high salt containing glycerine Technology of High Concentration OrganicWastewater Treatment, and high salt contains the vacancy of sodium-chlor and glycerine recovery technology in glycerine high concentrated organic wastewater, provide a kind of high salt containing sodium-chlor and glycerine recovery method in glycerine organic waste water.
The present invention includes following steps:
(1) adsorb
High salt by macroporous resin, makes the glycerol molecule in macroporous resin adsorption waste water containing glycerine high concentrated organic wastewater, obtains the absorption macroporous resin of glycerol molecule and the effluent liquid of sodium chloride-containing;
(2) evaporation concentration
The effluent liquid of step (1) absorption gained sodium chloride-containing is flowed into vaporizer by pipeline, evaporation concentration is carried out to the effluent liquid of sodium chloride-containing, obtains sodium-chlor concentrated solution;
(3) crystallization
Crystallization treatment is carried out to step (2) gained sodium-chlor concentrated solution, obtains the mother liquor after solid sodium chloride and crystallization filtration;
(4) dilution and biochemical treatment
Discharge after mother liquor dilution after step (3) crystallization is filtered and biochemical treatment;
(5) desorption
With the macroporous resin after desorbing agent rinse step (1) process, eluted by the glycerine be adsorbed on macroporous resin, obtain glycerinated elutriant, the macroporous resin after wash-out can drop in step (1) absorption and recycle;
(6) distill
Distill the glycerinated elutriant of gained after step (5) desorption, obtain desorbing agent and raw glycerine, desorbing agent can drop in step (5) desorption and recycle;
(7) fractionation
Fractionation is carried out to step (6) gained raw glycerine, obtains finished product glycerine and rectificated remaining liquid.
In step (1), described high salt can be 5% ~ 30% containing the mass percentage concentration of sodium-chlor in glycerine organic waste water, and the mass percentage concentration of glycerine can be 3% ~ 20%.
In step (2), described vaporizer can be selected from the one in thin-film evaporator, multiple-effect evaporator, circular form vaporizer etc.; The mass percentage concentration of described sodium-chlor concentrated solution can be 80% ~ 90%.
In step (5), described desorbing agent can adopt ethanol etc.
Compared with the prior art, the present invention has following outstanding advantages:
(1) by adsorption treatment, realize sodium-chlor and sweet oil separating, ensure the feasibility of subsequent evaporation concentration and distillation process.
(2) after adsorption treatment, the effluent liquid of sodium chloride-containing, after evaporation concentration and crystallization treatment, obtains sodium chloride crystal and crystalline mother solution, because salinity in mother liquor reduces, takes biochemical processing process, make water outlet water quality reaching standard after can diluting.
(3) after desorbing agent wash-out, the macroporous resin of gained can drop in adsorption treatment again and uses, and namely macroporous resin can recycle in the removal process of high salt containing sodium-chlor in glycerine high concentrated organic wastewater and glycerine.
(4) after desorbing agent wash-out, the glycerinated elutriant of gained processes through distillation, obtain desorbing agent, desorbing agent can drop in desorption process again and use, and namely desorbing agent can recycle in the removal process of high salt containing sodium-chlor in glycerine high concentrated organic wastewater and glycerine, forms resources conservation.
(5) after desorbing agent wash-out, the glycerinated elutriant of gained obtains finished product glycerine through distillation and fractionation process, and purity can reach 95%.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
The present invention is based on high salt containing the composition of glycerine high concentrated organic wastewater, character and existing processing scheme, devise a kind of high salt containing Glycerol Wastewater treatment process, it relates to the treatment process such as absorption, evaporation concentration, crystallization, biochemical treatment, desorption, distillation, fractionation, thus forms a kind of method that effectively can realize high salt and recycle containing sodium-chlor in Glycerol Wastewater and glycerine.
Referring to Fig. 1, the specific embodiment of the present invention is described.
Embodiment 1
With sodium-chlor and the certain density solution simulated wastewater of glycerol, waste water quality is in table 1.
The water quality situation of table 1 simulated wastewater
| Title | COD(ppm) | Chlorion (ppm) | Glycerine (%) | Sodium-chlor (%) |
| Simulated wastewater | 60908 | 121380 | 10.0 | 20.0 |
(1) adsorb
The content of simulated wastewater sodium-chlor, glycerine is respectively 20%, 10%, through macroporous resin adsorption, the content obtaining inhaling sodium-chlor, glycerine in remaining liquid is respectively 19.2%, 0.4%, and this illustrates that most glycerine is adsorbed on macroporous resin, realizes being separated of glycerine and sodium-chlor.
(2) evaporation concentration
Make to flow into vaporizer by the effluent liquid of step (1) absorption gained sodium chloride-containing by pipeline, evaporation concentration is carried out to the effluent liquid of sodium chloride-containing, obtains sodium-chlor concentrated solution.
Described vaporizer is thin-film evaporator, and sodium-chlor concentrated solution concentration is 86.3%.
(3) crystallization
Crystallization treatment is carried out to step (2) gained sodium-chlor concentrated solution, obtains the mother liquor after solid sodium chloride and crystallization filtration.The COD of mother liquor, glycerine, sodium chloride content are respectively 1679ppm, 0.78%, 0.4%.
(4) dilution and biochemical treatment
Discharge after mother liquor dilution after step (3) crystallization is filtered and biochemical treatment.Effluent quality COD, glycerine, sodium chloride content are respectively 43ppm, 0.004%, 0.013%.
(5) desorption
With the macroporous resin after desorbing agent rinse step (1) process, eluted by the glycerine be adsorbed on macroporous resin, obtain glycerinated elutriant and macroporous resin, macroporous resin drops in step (1) absorption and recycles.
Described desorbing agent is ethanol.In elutriant, the content of sodium-chlor, glycerine is respectively 0.5%, 9.47%
(6) distill
Distill the glycerinated elutriant of gained after step (5) desorption, obtain ethanol and raw glycerine, ethanol drops in step (5) desorption and recycles.In raw glycerine, glycerol content is 78.3%.
(7) fractionation
Fractionation is carried out to step (6) gained raw glycerine, obtains finished product glycerine and rectificated remaining liquid.The purity of finished product glycerine can reach 95.2%.
The test-results that sodium-chlor reclaims and glycerine reclaims as shown in tables 2 and 3.
The test-results that table 2 sodium-chlor reclaims
| Title | COD(ppm) | Chlorion (ppm) | Glycerine (%) | Sodium-chlor (%) |
| Inhale remaining liquid | 2435 | 116987 | 0.4 | 19.2 |
| Evaporation concentration liquid | 2978 | 525890 | 0.5 | 86.3 |
| Rear mother liquor is filtered in crystallization | 1679 | 2417 | 0.78 | 0.4 |
| Effluent quality after biochemical | 43 | 78 | 0.004 | 0.013 |
The test-results that table 3 glycerine reclaims
| Title | COD(ppm) | Chlorion (ppm) | Glycerine (%) | Sodium-chlor (%) |
| Elutriant | 57689 | 3041 | 9.47 | 0.5 |
| Distillate | 489085 | 24 | 78.3 | 0.004 |
| Liquid fractionation | 589766 | — | 95.2 | — |
Embodiment 2
The raw water quality of the petrochemical wastewater in certain chemical plant is in table 4.
The experimental result of table 4 petrochemical wastewater
(1) adsorb
Sodium-chlor, glycerine, GLD, 2 in the former water of petrochemical wastewater, the content of 3-DCH, MCH is respectively 21.2%, 9.47%, 0.04%, 0.012%, 0.01% through macroporous resin adsorption, obtain inhaling sodium-chlor in remaining liquid, glycerine, GLD, 2, the content of 3-DCH, MCH is respectively 20.1%, 0.25%, 0.01%, 0.003%, 0.002%, and this illustrates most glycerine, GLD, 2, the Adsorption of Organics such as 3-DCH, MCH, on macroporous resin, realize being separated of organism and sodium-chlor.
(2) evaporation concentration
Make to flow into vaporizer by the effluent liquid of step (1) absorption gained sodium chloride-containing by pipeline, evaporation concentration is carried out to the effluent liquid of sodium chloride-containing, obtains sodium-chlor concentrated solution.
Described vaporizer is multiple-effect evaporator, and sodium-chlor concentrated solution concentration is 89.2%.
(3) crystallization
Crystallization treatment is carried out to step (2) gained sodium-chlor concentrated solution, obtains the mother liquor after solid sodium chloride and crystallization filtration.The COD of mother liquor, glycerine, sodium chloride content are respectively 5567ppm, 0.38%, 0.37%.
(4) dilution and biochemical treatment
Discharge after mother liquor dilution after step (3) crystallization is filtered and biochemical treatment.Effluent quality COD, glycerine, sodium chloride content are respectively 58ppm, 0.002%, 0.012%.
(5) desorption
With the macroporous resin after desorbing agent rinse step (1) process, eluted by the glycerine be adsorbed on macroporous resin, obtain glycerinated elutriant and macroporous resin, macroporous resin drops in step (1) absorption and recycles.
Described desorbing agent is ethanol.In elutriant, the content of sodium-chlor, glycerine is respectively 0.98%, 9.19%
(6) distill
Distill the glycerinated elutriant of gained after step (5) desorption, obtain ethanol and raw glycerine, ethanol drops in step (5) desorption and recycles.In raw glycerine, glycerol content is 80.3%.
(7) fractionation
Fractionation is carried out to step (6) gained raw glycerine, obtains finished product glycerine and rectificated remaining liquid.The purity of finished product glycerine can reach 95.8%.
The test-results that table 5 sodium-chlor reclaims
| Title | COD(ppm) | Chlorion (ppm) | Glycerine (%) | Sodium-chlor (%) |
| Inhale remaining liquid | 5087 | 123980 | 20.1 | 0.25 |
| Evaporation concentration liquid | 10893 | 583823 | 89.2 | 0.42 |
| Rear mother liquor is filtered in crystallization | 5567 | 2356 | 0.37 | 0.38 |
| Effluent quality after biochemical | 58 | 82 | 0.012 | 0.002 |
The test-results that table 6 glycerine reclaims
| Title | COD(ppm) | Chlorion (ppm) | Glycerine (%) | Sodium-chlor (%) |
| Elutriant | 402347 | 5021 | 0.98 | 9.19 |
| Distillate | 484562 | 30 | 0.005 | 80.3 |
| Liquid fractionation | 549344 | — | — | 95.8 |
The test-results that sodium-chlor reclaims and glycerine reclaims as shown in table 5 and table 6.
Claims (5)
1. high salt is containing sodium-chlor and a glycerine recovery method in glycerine organic waste water, it is characterized in that comprising the following steps:
(1) adsorb
Make high salt contain glycerine high concentrated organic wastewater by macroporous resin, make the glycerol molecule in macroporous resin adsorption waste water, obtain the absorption macroporous resin of glycerol molecule and the effluent liquid of sodium chloride-containing;
(2) evaporation concentration
Make to flow into vaporizer by the effluent liquid of step (1) absorption gained sodium chloride-containing by pipeline, evaporation concentration is carried out to the effluent liquid of sodium chloride-containing, obtains sodium-chlor concentrated solution;
(3) crystallization
Crystallization treatment is carried out to step (2) gained sodium-chlor concentrated solution, obtains the mother liquor after solid sodium chloride and crystallization filtration;
(4) dilution and biochemical treatment
Discharge after mother liquor dilution after step (3) crystallization is filtered and biochemical treatment;
(5) desorption
With the macroporous resin after desorbing agent rinse step (1) process, eluted by the glycerine be adsorbed on macroporous resin, obtain glycerinated elutriant, the macroporous resin after wash-out can drop in step (1) absorption and recycle;
(6) distill
Distill the glycerinated elutriant of gained after step (5) desorption, obtain desorbing agent and raw glycerine, desorbing agent can drop in step (5) desorption and recycle;
(7) fractionation
Fractionation is carried out to step (6) gained raw glycerine, obtains finished product glycerine and rectificated remaining liquid.
2. a kind of high salt contains sodium-chlor and glycerine recovery method in glycerine organic waste water as claimed in claim 1, it is characterized in that in step (1), described high salt is 5% ~ 30% containing the mass percentage concentration of sodium-chlor in glycerine organic waste water, and the mass percentage concentration of glycerine is 3% ~ 20%.
3. a kind of high salt, containing sodium-chlor and glycerine recovery method in glycerine organic waste water, is characterized in that, in step (2), described vaporizer is selected from the one in thin-film evaporator, multiple-effect evaporator, circular form vaporizer as claimed in claim 1.
4. a kind of high salt is containing sodium-chlor and glycerine recovery method in glycerine organic waste water as claimed in claim 1, and it is characterized in that in step (2), the mass percentage concentration of described sodium-chlor concentrated solution is 80% ~ 90%.
5. a kind of high salt, containing sodium-chlor and glycerine recovery method in glycerine organic waste water, is characterized in that, in step (5), described desorbing agent is ethanol as claimed in claim 1.
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Cited By (14)
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| CN105347363A (en) * | 2015-11-26 | 2016-02-24 | 山东潍坊润丰化工股份有限公司 | Process for treating byproduct industrial salt by water-washing adsorption method |
| CN105585423A (en) * | 2015-12-02 | 2016-05-18 | 浙江奇彩环境科技股份有限公司 | Improved glycerol production technology |
| CN105836764A (en) * | 2016-03-24 | 2016-08-10 | 南京理工大学 | Recycling method of waste salt from salt-containing waste water in organic synthetic industry |
| CN106830569A (en) * | 2017-03-31 | 2017-06-13 | 山西翔宇化工有限公司 | A kind of processing method of salt organic waste water high |
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| CN113429032A (en) * | 2021-06-01 | 2021-09-24 | 浙江工业大学 | Treatment method of high-salt high-COD wastewater |
| CN114590948A (en) * | 2022-04-26 | 2022-06-07 | 扬州大学 | Harmless treatment and resource utilization process for epoxy resin production wastewater |
| CN115417549A (en) * | 2022-09-02 | 2022-12-02 | 寿光永康化学工业有限公司 | Comprehensive treatment process for high-salinity organic wastewater |
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