CN103787542A - Process and device for recovering and treating wastewater generated by preparing sebacic acid with castor oil - Google Patents
Process and device for recovering and treating wastewater generated by preparing sebacic acid with castor oil Download PDFInfo
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- CN103787542A CN103787542A CN201410042559.0A CN201410042559A CN103787542A CN 103787542 A CN103787542 A CN 103787542A CN 201410042559 A CN201410042559 A CN 201410042559A CN 103787542 A CN103787542 A CN 103787542A
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- castor oil
- sebacic acid
- waste water
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- 239000002351 wastewater Substances 0.000 title claims abstract description 70
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000004359 castor oil Substances 0.000 title claims abstract description 27
- 235000019438 castor oil Nutrition 0.000 title claims abstract description 27
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 title claims abstract description 27
- 238000002425 crystallisation Methods 0.000 claims abstract description 41
- 230000008025 crystallization Effects 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000011084 recovery Methods 0.000 claims abstract description 21
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000002699 waste material Substances 0.000 claims abstract description 20
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 230000001105 regulatory effect Effects 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000002360 preparation method Methods 0.000 claims description 26
- 239000002002 slurry Substances 0.000 claims description 22
- 239000002253 acid Substances 0.000 claims description 20
- 150000002632 lipids Chemical class 0.000 claims description 20
- 238000009833 condensation Methods 0.000 claims description 19
- 230000005494 condensation Effects 0.000 claims description 19
- 239000012452 mother liquor Substances 0.000 claims description 19
- 229940056729 sodium sulfate anhydrous Drugs 0.000 claims description 19
- 238000001704 evaporation Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 17
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 17
- 235000011152 sodium sulphate Nutrition 0.000 claims description 17
- 229960003010 sodium sulfate Drugs 0.000 claims description 16
- 230000008020 evaporation Effects 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 13
- 238000000746 purification Methods 0.000 claims description 10
- 238000004064 recycling Methods 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 9
- 238000012856 packing Methods 0.000 claims description 7
- 238000006124 Pilkington process Methods 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000001471 micro-filtration Methods 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 abstract 2
- 229930195729 fatty acid Natural products 0.000 abstract 2
- 239000000194 fatty acid Substances 0.000 abstract 2
- 150000004665 fatty acids Chemical class 0.000 abstract 2
- 239000000356 contaminant Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 31
- 238000000605 extraction Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- WBHHMMIMDMUBKC-QJWNTBNXSA-N ricinoleic acid Chemical compound CCCCCC[C@@H](O)C\C=C/CCCCCCCC(O)=O WBHHMMIMDMUBKC-QJWNTBNXSA-N 0.000 description 5
- 229960003656 ricinoleic acid Drugs 0.000 description 5
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002207 thermal evaporation Methods 0.000 description 3
- ZEMPKEQAKRGZGQ-AAKVHIHISA-N 2,3-bis[[(z)-12-hydroxyoctadec-9-enoyl]oxy]propyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(O)CCCCCC)COC(=O)CCCCCCC\C=C/CC(O)CCCCCC ZEMPKEQAKRGZGQ-AAKVHIHISA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 231100001261 hazardous Toxicity 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical group [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
Images
Abstract
The invention relates to a process and a device for recovering and treating wastewater generated by preparing sebacic acid with castor oil. The process comprises the steps of a, adjusting the pH value, b, purifying a fatty acid, c, carrying out evaporative crystallization, d, carrying out solid-liquid separation of anhydrous sodium sulfate, e, purifying secondary steam by removing phenol, f, compressing the secondary steam, and g, repeating the steps c-f, and collecting a sodium phenate solution, condensate water and the separated solid obtained in the step d. The invention also relates to a device for recovering and treating wastewater generated by preparing sebacic acid with castor oil; the device comprises a pH regulating reservoir, a fatty acid purifier, a waste material delivery pump, a mechanical steam recompression/evaporative crystallization system, a dryer and the like. The recovery process is simple to operate and low in cost, and also capable of realizing zero emission of contaminants, and environment-friendly and energy-saving, and in the meantime, the recovery device is simple and easy to operate.
Description
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Technical field
The present invention relates to a kind of wastewater recycling process and device, be specifically related to wastewater recovery processing technique and device that a kind of Viscotrol C sebacic acid processed produces.
Background technology
Take Viscotrol C as raw material, in by hydrolysis, using phenol as the production process of the technique sebacic acid processed such as catalyzer alkali thermo-cracking, neutralization, decolouring, acidifying, can produce a large amount of waste water, the waste water and the waste water that produce approximately 30 tons are had following feature by 1 ton of sebacic acid of every production: sodium sulfate 30-350g/L, phenol 100-5000mg/L, lipid acid impurity 50--25000 mg/L, COD5000--15000mg/L, pH value 2-5.This waste water contains the sodium sulfate to human body and the poisonous and hazardous phenol of environment and high density, belongs to extremely unmanageable containing phenol brine waste.If directly discharge, will cause serious destruction to environment.If phenol and sodium sulfate are separated to individual curing, except processing cost is high, also cause the waste of useful resources, increase the production cost of enterprise.
Application number is the application for a patent for invention file of CN102372378A, discloses the treatment process of the waste water of a kind Preparation of Sebacic Acid From Castor Oil generation: first iron filings are added to oxidation pond, form the fixed bed of solid; Then the waste water of removing after filtration after solid sundries is entered to oxidation pond, the hydrogen peroxide oxidant that is simultaneously 30% by concentration adds oxidation pond; By blower fan, air is sent into oxidation pond; Finally adding sulfuric acid and regulating pH value is 3～4, carries out triphase catalytic oxidation reaction, and wherein catalyst activity component is ferrous sulfate, and temperature of reaction is 50 ℃～60 ℃, and the reaction times is 4h～8h; After having reacted, waste water after treatment is entered to wastewater equalization pond, and add flocculation agent, then filter and remove suspended substances precipitation, the waste water that obtains handling well.
Aforesaid method has been brought new impurity into liquid waste disposal, also needs to expend sulfuric acid, hydrogen peroxide etc. simultaneously, has increased cost, and the suspended substance comparison of ingredients complexity simultaneously generating needs further to process and reclaim.In order to make recovery process simpler, reduce cost recovery, publication number is the application for a patent for invention file of 101139148A, a kind for the treatment of process and special extractor thereof of sebacic acid factory effluent are disclosed: adopt ricinolic acid to extract and prohibit row's thing as extraction agent, and by special multi-stage solvent extraction device cyclical operation, realization taboo row thing separates with discharge water.
Publication number is the application for a patent for invention file of 101654305A, and a kind of extracting, evaporating crystallization coupling resource utilization is containing phenol nitre liquid technique.Mainly comprise the following steps: A, Wastewater Pretreatment, first enter in cooling pool (1) containing phenol nitre liquid, because the sebacic acid of cooling crystallization returns in sebacic acid preparation technology purifying again, supernatant liquid in cooling pool (1) enters a pH value equalizing tank (2), regulating the pH value of waste water is 3-7, then will squeeze in extraction tower (6) containing phenol nitre liquid by the first water pump (3), B, phenol extraction is entered by the top of extraction tower (6) containing phenol nitre liquid, ricinolic acid is entered by extraction tower (6) bottom, by counter-current operation, profit two-phase is fully contacted, discharge containing phenol ricinolic acid at extraction tower (6) top, enter in the first water-and-oil separator (7), what discharged at the first water-and-oil separator (7) top returns the cleavage step in sebacic acid preparation technology containing phenol ricinolic acid, the organism that discharge the first water-and-oil separator (7) bottom goes back to extraction tower (6) top, reflux ratio is 1: 1 to 1: 8, waste water after dephenolize is escaped and enter in the second water-and-oil separator (8) by extraction tower (6) bottom, the isolated solution containing ricinolic acid goes back to extraction tower (6) bottom by the second water-and-oil separator (8) top, reflux ratio is 1: 1 to 1: 8, dephenolize is discharged by the second water-and-oil separator (8) bottom containing nitre waste water, the dephenolize that C, triple effect evaporation crystallization are discharged from the second water-and-oil separator (8) bottom enters the 2nd pH value equalizing tank (9) containing nitre waste water, regulating the pH value of waste water is 8-13, then enters triple effect evaporation crystallizer by the second water pump (10) and carries out evaporative crystallization, the sodium sulfate magma that D, reclaim(ed) sulfuric acid sodium are discharged by the first crystallizer (12), the second crystallizer (14), the 3rd crystallizer (16) bottom enters sodium sulfate magma storage tank (20) and precipitates, the sodium sulfate magma of discharging from sodium sulfate magma storage tank (20) bottom is by the centrifugation of whizzer (21), dry in moisture eliminator (22), thus sodium sulfate pressed powder obtained.
But aforesaid method, substantially be to adopt extraction agent to extract phenol, need to add extraction agent, give in waste water and brought new impurity, the pervaporation simultaneously adopting or triple effect evaporation method need to provide the heat energy of a large amount of generation steam, and retrieving arrangement is wherein too complicated.
Summary of the invention
In order to solve the waste water reclamation treatment process high cost of existing Preparation of Sebacic Acid From Castor Oil generation and can to bring the problems such as new impurity into, the invention provides a kind of low power consuming, reclaim product purity recovery processing technique high, simple to operate, the waste-water recovering treater that the present invention simultaneously also provides a kind of Preparation of Sebacic Acid From Castor Oil to produce.
For addressing the above problem, the technical solution adopted in the present invention is as follows:
The wastewater recovery processing technique that Preparation of Sebacic Acid From Castor Oil produces, comprises the steps:
A. regulate pH value: in waste water, add sodium hydroxide, regulating pH value is 8-13, and this step can be carried out in various large containers, and as pH regulator pond, described waste water is produced by Preparation of Sebacic Acid From Castor Oil, and described waste water contains sodium sulfate, phenol and lipid acid impurity; Described waste water is adding after sodium hydroxide, lipid acid generation saponification reaction.
B. lipid acid purifies: by waste water process air-float method or the processing of micro-filtration method through a step process, the vesicle that waste liquid height of formation disperses, form water-gas-particle three-phase mixed system, sodium soap is attached on bubble and floats to the water surface and forms scum layer, then scrape off scum layer, remove lipid acid impurity, this step can be carried out in the lipid acid purifier devices such as air floatation machine.
C. evaporative crystallization: by the waste water through b step process in function of mechanical steam recompression system to evaporate and crystallization treatment at the temperature of 50-120 ℃, obtain Sodium sulfate anhydrous.min(99) slurries, secondary steam and water of condensation.In secondary steam, contain phenol.
D. Sodium sulfate anhydrous.min(99) slurries solid-liquid separates: the Sodium sulfate anhydrous.min(99) slurries that obtain through c step are carried out to solid-liquid separation processing, this solid-liquid separation processing can adopt the devices such as whizzer to carry out, obtain the solid and the liquid separating that separate, then isolated liquid is imported in the function of mechanical steam recompression evaporation and crystallization system in c step by pump;
E. secondary steam removes phenol purification: the secondary steam obtaining through c step is passed in steam purifier and carries out purifying treatment, in described steam purifier, be added with sodium hydroxide solution, obtain the secondary steam of sodium phenylate solution and purification;
F. secondary steam compression: the secondary steam of the purification obtaining through e step process is carried out to processed compressed, then pass in function of mechanical steam recompression system, as the thermal source of evaporation;
Waste water is main in function of mechanical steam recompression evaporation and crystallization system there is following change procedure: 1. at the heating chamber of vaporizer, after steam source and wastewater heat exchange, become water of condensation, and waste water is subject to thermal evaporation, time part changes secondary steam into, waste water is concentrated simultaneously; 2. secondary steam is first except compress to improve again temperature, the then thermal source of conduct evaporation of pressure of steam after phenol purification through vapour compressor.Owing to containing a large amount of phenol in secondary steam, for guaranteeing the water quality of water of condensation and reducing water of condensation is removed to phenol processing again, so must remove phenol to secondary steam purifies, utilize sodium hydroxide and phenol generation chemical reaction to generate the principle of sodium phenylate, scavenging agent with sodium hydroxide as phenol in secondary steam, reclaims sodium phenylate; 3. waste water is constantly by evaporation concentration, when the sodium sulfate concentration in waste water exceedes it at that time when the saturation concentration at temperature, the continuous crystallization of sodium sulfate and formation particulate state sodium sulfate (Sodium sulfate anhydrous.min(99)) crystal not of uniform size of growing up, crystal forms Sodium sulfate anhydrous.min(99) slurry in the enrichment of the bottom of crystallizer under the effect of deadweight.
G. repeating step c-f at least one times, then collects the solid separating that sodium phenylate solution, water of condensation and d step obtain.Carry out this step, after concentrated Sodium sulfate anhydrous.min(99) slurries centrifugation, mother liquor is continued to return in evaporative crystallizer, then along with importing to heating chamber top by concentrated solution recycle pump, the waste liquid in evaporative crystallizer realizes circulation, and during realize heat exchange when the heating chamber, be subject to thermal evaporation further to carry out condensing crystal, circulation repeatedly makes the sulfate crystal in waste water separate out; The phenol containing in secondary steam generates sodium phenylate after by sodium hydroxide solution, and steam makes the phenol overwhelming majority in secondary steam be absorbed by sodium hydroxide solution after repeatedly circulating
In the present invention, preferably, the solid of the separation of g collection step is carried out to drying treatment, make dry Sodium sulfate anhydrous.min(99), then pack;
In the present invention, preferably, the sodium phenylate solution of g collection step is reclaimed.
In the present invention, preferably, the water of condensation that described c step is obtained carries out heat exchange with the waste water being produced by Preparation of Sebacic Acid From Castor Oil by interchanger, then by the condensation water collection after heat exchange.
A device for the waste water reclamation processing that Preparation of Sebacic Acid From Castor Oil produces, comprises as lower device:
PH regulator pond, lipid acid cleaner, waste material transferpump and function of mechanical steam recompression evaporation and crystallization system; The discharge port in described pH regulator pond is connected with lipid acid cleaner and waste material transferpump successively by pipeline;
Described function of mechanical steam recompression evaporation and crystallization system comprises: evaporative crystallizer, concentrated solution recycle pump, whizzer, vacuum pump, steam purifier, vapour compressor, the heating chamber that described evaporative crystallizer comprises evaporative crystallization chamber and is connected with its upper opening, described heating chamber is provided with the first opening for feed, the first discharge port, secondary heat source entrance and condensation-water drain, bottom, described evaporative crystallization chamber is provided with slurry outlet and whizzer mother liquor refluxing opening, and the sidewall of described evaporative crystallization chamber is provided with the second opening for feed, secondary steam outlet, described slurry outlet is connected with whizzer by pipeline, and described whizzer is provided with slurry entrance, whizzer mother liquor outlet and solid discharge port, described whizzer mother liquor outlet by pipeline successively with whizzer mother liquor reflux pump, the whizzer mother liquor refluxing opening of bottom, evaporative crystallization chamber connects, and described concentrated solution recycle pump is carried pump outlet with waste material respectively by threeway and/or by-pass line, the first opening for feed on heating chamber, the second opening for feed of evaporative crystallization chamber sidewall connects, the outlet of described secondary steam by pipeline successively with vacuum pump, steam purifier, vapour compressor is connected with secondary heat source entrance.Evaporative crystallizer can be large container.
Preferably, the solid discharge port of described whizzer is connected with dry packing machine by pipeline.
Preferably, described condensation-water drain is connected with recycling condensing water pump by pipeline.
Preferably, described secondary steam cleaner is provided with a solution discharge port, and described solution discharge port is connected with sodium phenylate solution recovery pump by pipeline.
Preferably, on described pipeline, be equipped with valve.
The invention provides wastewater recovery processing technique and device that a kind of Preparation of Sebacic Acid From Castor Oil produces, compared to prior art, there is following technique effect:
In function of mechanical steam recompression evaporation and crystallization system, after concentrated Sodium sulfate anhydrous.min(99) slurries centrifugation, mother liquor is continued to return in evaporative crystallizer, then along with importing to heating chamber top by concentrated solution recycle pump, the waste liquid in evaporative crystallizer realizes circulation, and during realize heat exchange when the heating chamber, be subject to thermal evaporation further to carry out condensing crystal, circulation repeatedly makes the sulfate crystal in waste water separate out; The phenol containing in secondary steam generates sodium phenylate after by sodium hydroxide solution, and steam makes the phenol overwhelming majority in secondary steam be absorbed by sodium hydroxide solution after repeatedly circulating; Then, the steam of purification passes into the heat exchanger in heating chamber after being compressed, heated up by vapour compressor, and the water of condensation that steam heat release condensation forms can be collected utilization; Then collect reuse Sodium sulfate anhydrous.min(99), sodium phenylate solution and water of condensation, realized the resource utilization reuse of waste water and the zero release of poisonous and harmful waste water, not only reduced production cost but also protected environment.
Evaporative crystallization Treatment for Reuse by function of mechanical steam recompression system to waste water, the interpolation of not bringing other compositions in existing recovery process into, has reduced processing step and extraction cost; In the present invention, adopt function of mechanical steam recompression technology to concentrate waste liquid, only need to use relatively few energy, the i.e. mechanical energy of the compressor impeller in compressing hot pump situation, energy is added in technique heating medium and enters continuous circulation, has significantly reduced the required energy consumption of recovery process; In addition, the recycling and processing device in the present invention, equipment is simpler, easy to operate compared with legacy equipment.
Below in conjunction with the drawings and the specific embodiments, the present invention is described in further detail.
Accompanying drawing explanation
Further illustrate the embodiment of the present invention below in conjunction with accompanying drawing.
Fig. 1 is the waste-water recovering treater that Preparation of Sebacic Acid From Castor Oil produces
Accompanying drawing explanation: 1, PH equalizing tank; 2, lipid acid cleaner; 21, waste liquid transferpump; 3, evaporative crystallizer 3; 31, concentrated solution recycle pump; 32, evaporative crystallization chamber; 321, the second opening for feed; 322, slurry outlet; 323, whizzer mother liquor refluxing opening; 324, secondary steam outlet; 33, heating chamber; 331, secondary heat source entrance; 332, condensation-water drain; 333, the first opening for feed; 334, the first discharge port; 4, whizzer; 41, centrifuge mother liquor reflux pump; 5, dry packing machine; 6, steam purifier; 7, vapour compressor; 8, sodium phenylate solution recovery pump; 9, recycling condensing water pump; 10, vacuum pump.
Embodiment
Embodiment 1
The waste water reclamation that 1 ton of Preparation of Sebacic Acid From Castor Oil is produced, through detecting, contriver records sodium sulfate 150g/L in this waste water, phenol 2000mg/L, lipid acid impurity 5000mg/L, COD8500mg/L, pH value 2.8.For this batch of waste liquid, adopt and recycle as lower device:
A device for the waste water reclamation processing that Preparation of Sebacic Acid From Castor Oil produces, comprises as lower device:
PH regulator pond 1, lipid acid cleaner 2, waste material transferpump 21, dry packing machine 5, recycling condensing water pump 9, sodium phenylate solution recovery pump 8 and function of mechanical steam recompression evaporation and crystallization system;
The discharge port in described pH regulator pond 1 is connected with lipid acid cleaner 2 and waste material transferpump 21 successively by pipeline;
Described function of mechanical steam recompression evaporation and crystallization system comprises: evaporative crystallizer 3, concentrated solution recycle pump 31, whizzer 4, vacuum pump 10, steam purifier 6, vapour compressor 7, the heating chamber 33 that described evaporative crystallizer 3 comprises evaporative crystallization chamber 32 and is connected with its upper opening, described heating chamber 33 is provided with the first opening for feed 333, the first discharge port 334, secondary heat source entrance 331 and condensation- water drain 332,32 bottoms, described evaporative crystallization chamber are provided with slurry outlet 322 and whizzer mother liquor refluxing opening 323, and the sidewall of described evaporative crystallization chamber 32 is provided with the second opening for feed 321, secondary steam outlet 324, described slurry outlet 322 is connected with whizzer 4 by pipeline, and described whizzer 4 is provided with slurry entrance, whizzer mother liquor outlet and solid discharge port, described whizzer mother liquor outlet by pipeline successively with whizzer mother liquor reflux pump 41, the whizzer mother liquor refluxing opening 323 of evaporative crystallization chamber bottom connects, described concentrated solution recycle pump 31 by three-way pipeline and by-pass line respectively with the outlet of waste material transferpump 21, the first opening for feed 333 on heating chamber 33, the second opening for feed 321 of evaporative crystallization chamber 32 sidewalls connects, the outlet 324 of described secondary steam by pipeline successively with vacuum pump 10, steam purifier 6, vapour compressor 7 is connected with secondary heat source entrance 321.
The solid discharge port of described whizzer 4 is connected with dry packing machine 5 by pipeline, described condensation-water drain 332 is connected with recycling condensing water pump 9 by pipeline, described steam purifier 6 is provided with a solution discharge port, and described solution discharge port is connected with sodium phenylate solution recovery pump 8 by pipeline.On described pipeline, be equipped with valve.
Recycling step is as follows:
A. regulate pH value: waste water is added in pH regulator pond 1, then in waste water, add sodium hydroxide, regulating pH value is 8-13, and described waste water is produced by Preparation of Sebacic Acid From Castor Oil, and described waste water contains sodium sulfate, phenol and lipid acid impurity;
B. lipid acid purifies: the waste water through b step process is added to process air-float method processing lipid acid cleaner 2 from the discharge port in pH regulator pond 1 by pipeline, scrape off scum layer;
C. evaporative crystallization: will add to by waste material transferpump 21 in the evaporative crystallization chamber 32 of the evaporative crystallizer 3 in function of mechanical steam recompression system through the waste water of c step process, then to evaporate and crystallization treatment at the temperature of 50-120 ℃, obtain Sodium sulfate anhydrous.min(99) slurries, secondary steam and water of condensation;
D. Sodium sulfate anhydrous.min(99) slurries solid-liquid separates: the Sodium sulfate anhydrous.min(99) slurries that obtain through c step are carried out to solid-liquid separation processing by whizzer 4, obtain the solid and the liquid separating of separation, then isolated liquid is pumped in the function of mechanical steam recompression system in c step;
E. secondary steam purifies except phenol: the secondary steam obtaining through c step is passed into vacuum pump 10 and be transported in steam purifier 6 and carry out purifying treatment, in described steam purifier 6, be added with sodium hydroxide solution, obtain the secondary steam of sodium phenylate solution and purification;
F. secondary steam compression: the secondary steam of the purification obtaining through e step process is carried out to processed compressed by vapour compressor 7, then pass in function of mechanical steam recompression system;
G. repeating step c-f, then collects the solid separating that sodium phenylate solution, water of condensation and d step obtain, and then the solid of the separation of collecting is dried and obtains dry Sodium sulfate anhydrous.min(99) through dry packing machine 5, then obtains product through packing; Sodium phenylate solution is collected by sodium phenylate solution recovery pump 8; Water of condensation is passed through to 9 recyclings of recycling condensing water pump.
Sodium sulfate anhydrous.min(99) after reclaiming is detected, and sodium sulphate content is greater than 98.5%, is qualified industrial II level Sodium sulfate anhydrous.min(99); In water of condensation, the concentration of phenol is 0.05mg/L after testing, and decontamination effect improving is good, and water of condensation is gradable to be back in production.Can find out, after the present invention program processes, the separated and reuse of material lipid acid, phenol and sodium sulfate in waste liquid, Treatment for Reuse is respond well, has substantially realized the zero release of hazardous and noxious substances.
Above-mentioned embodiment is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (9)
1. the wastewater recovery processing technique that Preparation of Sebacic Acid From Castor Oil produces, is characterized in that comprising the steps:
A. regulate pH value: in waste water, add sodium hydroxide, regulating pH value is 8-13, and described waste water is produced by Preparation of Sebacic Acid From Castor Oil, and described waste water contains sodium sulfate, phenol and lipid acid impurity;
B. lipid acid purifies: the waste water through a step process, through air-float method or the processing of micro-filtration method, is removed to removing dross;
C. evaporative crystallization: by the waste water through b step process in function of mechanical steam recompression system to evaporate and crystallization treatment at the temperature of 50-120 ℃, obtain Sodium sulfate anhydrous.min(99) slurries, secondary steam and water of condensation;
D. Sodium sulfate anhydrous.min(99) slurries solid-liquid separates: the Sodium sulfate anhydrous.min(99) slurries that obtain through c step are carried out to solid-liquid separation processing, obtain the solid and the liquid separating that separate, then isolated liquid is imported in the function of mechanical steam recompression evaporation and crystallization system in c step by pump;
E. secondary steam removes phenol purification: the secondary steam obtaining through c step is passed in steam purifier and carries out purifying treatment, in described steam purifier, be added with sodium hydroxide solution, obtain the secondary steam of sodium phenylate solution and purification;
F. secondary steam compression: the secondary steam of the purification obtaining through e step process is carried out to processed compressed, then pass in function of mechanical steam recompression system;
G. repeating step c-f at least one times, then collects the solid separating that sodium phenylate solution, water of condensation and d step obtain.
2. the wastewater recovery processing technique that Preparation of Sebacic Acid From Castor Oil according to claim 1 produces, is characterized in that: the solid of the separation of g collection step is carried out to drying treatment, make dry Sodium sulfate anhydrous.min(99), then pack.
3. the wastewater recovery processing technique that Preparation of Sebacic Acid From Castor Oil according to claim 1 produces, is characterized in that: the sodium phenylate solution of g collection step is reclaimed.
4. the wastewater recovery processing technique that Preparation of Sebacic Acid From Castor Oil according to claim 1 produces, it is characterized in that: the water of condensation that described c step is obtained carries out heat exchange with the waste water being produced by Preparation of Sebacic Acid From Castor Oil by interchanger, then by the condensation water collection after heat exchange.
5. a device for the waste water reclamation processing that Preparation of Sebacic Acid From Castor Oil produces, is characterized in that comprising as lower device:
PH regulator pond, lipid acid cleaner, waste material transferpump and function of mechanical steam recompression evaporation and crystallization system; The discharge port in described pH regulator pond is connected with lipid acid cleaner and waste material transferpump successively by pipeline;
Described function of mechanical steam recompression evaporation and crystallization system comprises: evaporative crystallizer, concentrated solution recycle pump, whizzer, vacuum pump, steam purifier, vapour compressor, the heating chamber that described evaporative crystallizer comprises evaporative crystallization chamber and is connected with its upper opening, described heating chamber is provided with the first opening for feed, the first discharge port, secondary heat source entrance and condensation-water drain, bottom, described evaporative crystallization chamber is provided with slurry outlet and whizzer mother liquor refluxing opening, and the sidewall of described evaporative crystallization chamber is provided with the second opening for feed, secondary steam outlet, described slurry outlet is connected with whizzer by pipeline, and described whizzer is provided with slurry entrance, whizzer mother liquor outlet and solid discharge port, described whizzer mother liquor outlet by pipeline successively with whizzer mother liquor reflux pump, the whizzer mother liquor refluxing opening of bottom, evaporative crystallization chamber connects, and described concentrated solution recycle pump is carried pump outlet with waste material respectively by three-way pipeline and/or by-pass line, the first opening for feed on heating chamber, the second opening for feed of evaporative crystallization chamber sidewall connects, the outlet of described secondary steam by pipeline successively with vacuum pump, steam purifier, vapour compressor is connected with secondary heat source entrance.
6. the device of the waste water reclamation processing that Preparation of Sebacic Acid From Castor Oil according to claim 5 produces, is characterized in that: the solid discharge port of described whizzer is connected with dry packing machine by pipeline.
7. the device of the waste water reclamation processing that Preparation of Sebacic Acid From Castor Oil according to claim 5 produces, is characterized in that: described condensation-water drain is connected with recycling condensing water pump by pipeline.
8. the device of the waste water reclamation processing that Preparation of Sebacic Acid From Castor Oil according to claim 5 produces, is characterized in that: described steam purifier is provided with a solution discharge port, described solution discharge port is connected with sodium phenylate solution recovery pump by pipeline.
9. the device of the waste water reclamation processing producing according to the Preparation of Sebacic Acid From Castor Oil described in claim 5-8 any one, is characterized in that: on described pipeline, be equipped with valve.
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| CN107324578A (en) * | 2017-08-18 | 2017-11-07 | 武汉凯迪水务有限公司 | A kind of shale gas produced water treatment system and method |
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| CN109179745A (en) * | 2018-08-29 | 2019-01-11 | 杭州轩辉环境设备有限公司 | A kind for the treatment of process for the waste water producing fatty acid generation |
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Denomination of invention: Process and device for recovering and treating wastewater generated by preparing sebacic acid with castor oil Effective date of registration: 20181228 Granted publication date: 20150930 Pledgee: Bank of China Limited by Share Ltd. Guangzhou Panyu branch Pledgor: GUANGZHOU SINPURELY ENERGY CONSERVATION & ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Registration number: 2018440000409 |
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Granted publication date: 20150930 Pledgee: Bank of China Limited by Share Ltd. Guangzhou Panyu branch Pledgor: GUANGZHOU SINPURELY ENERGY CONSERVATION & ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Registration number: 2018440000409 |