CN103787542B - The wastewater recovery processing technique that a kind of Preparation of Sebacic Acid From Castor Oil produces and device - Google Patents
The wastewater recovery processing technique that a kind of Preparation of Sebacic Acid From Castor Oil produces and device Download PDFInfo
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- CN103787542B CN103787542B CN201410042559.0A CN201410042559A CN103787542B CN 103787542 B CN103787542 B CN 103787542B CN 201410042559 A CN201410042559 A CN 201410042559A CN 103787542 B CN103787542 B CN 103787542B
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- 239000002351 wastewater Substances 0.000 title claims abstract description 66
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000004359 castor oil Substances 0.000 title claims abstract description 23
- 235000019438 castor oil Nutrition 0.000 title claims abstract description 23
- 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 23
- 238000011084 recovery Methods 0.000 title claims abstract description 23
- 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 35
- 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
- 239000002002 slurry Substances 0.000 claims abstract description 23
- 238000001704 evaporation Methods 0.000 claims abstract description 21
- 238000009833 condensation Methods 0.000 claims abstract description 20
- 230000005494 condensation Effects 0.000 claims abstract description 20
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 claims abstract description 20
- 229940056729 sodium sulfate anhydrous Drugs 0.000 claims abstract description 20
- 239000002699 waste material Substances 0.000 claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 18
- 238000000746 purification Methods 0.000 claims abstract description 17
- 230000008020 evaporation Effects 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 15
- 150000002632 lipids Chemical class 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 230000006835 compression Effects 0.000 claims abstract description 5
- 238000007906 compression Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 239000012452 mother liquor Substances 0.000 claims description 19
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 16
- 235000011152 sodium sulphate Nutrition 0.000 claims description 16
- 229960003010 sodium sulfate Drugs 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 9
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 7
- 239000000194 fatty acid Substances 0.000 claims description 7
- 229930195729 fatty acid Natural products 0.000 claims description 7
- 150000004665 fatty acids Chemical class 0.000 claims description 7
- 238000006124 Pilkington process Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 238000001471 micro-filtration Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 31
- 238000000605 extraction Methods 0.000 description 12
- 238000004064 recycling Methods 0.000 description 12
- 239000003921 oil Substances 0.000 description 8
- 230000000694 effects Effects 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
- 238000007254 oxidation reaction Methods 0.000 description 5
- 238000012856 packing 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
- 238000004519 manufacturing 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
- 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
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001105 regulatory effect Effects 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
- 230000015572 biosynthetic process Effects 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
- 239000006185 dispersion Substances 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
- 231100001261 hazardous Toxicity 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
- 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
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 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
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
Landscapes
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The present invention relates to the wastewater recovery processing technique that a kind of Preparation of Sebacic Acid From Castor Oil produces, comprise the steps: a. adjust ph; B. lipid acid purification; C. evaporative crystallization; D. Sodium sulfate anhydrous.min(99) slurries solid-liquid separation; E. secondary steam is except phenol purification; F. secondary steam compression; G. repeating step c-f, then collects sodium phenylate solution, the solid be separated that water of condensation obtains with Step d.The invention still further relates to the waste-water recovering treater that a kind of Preparation of Sebacic Acid From Castor Oil produces, comprise as lower device: the devices such as pH regulator pond, lipid acid cleaner, waste material transferpump, function of mechanical steam recompression evaporation and crystallization system and drying machine.Recovery process of the present invention, simple to operate, cost is low, and the zero release of pollution substance can be realized, environmental protection and energy saving, retrieving arrangement is simple, easy to operate simultaneously.
Description
Technical field
The present invention relates to a kind of wastewater recycling process and device, be specifically related to wastewater recovery processing technique and the device of the generation of a kind of Viscotrol C sebacic acid.
Background technology
Take Viscotrol C as raw material, by hydrolysis, a large amount of waste water can be produced using phenol in the production process of the technique sebacic acid such as catalyzer alkali thermo-cracking, neutralization, decolouring, acidifying, often produce 1 ton of sebacic acid by the waste water of generation about 30 tons and waste water has following feature: sodium sulfate 30-350g/L, phenol 100-5000mg/L, fatty acid impurities 50--25000 mg/L, COD5000--15000mg/L, pH value 2-5.This waste water contains the sodium sulfate of phenol and the high density be harmful to human body and environmental toxic, belongs to extremely unmanageable containing phenol brine waste.If directly discharged, cause serious destruction by environment.If phenol and sodium sulfate are separated individual curing, except processing cost is high, also cause the waste of useful resources, add 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 that a kind Preparation of Sebacic Acid From Castor Oil produces: first iron filings are added oxidation pond, forms the fixed bed of solid; Then enter oxidation pond by removing the waste water after solid sundries after filtration, be that the hydrogen peroxide oxidant of 30% adds oxidation pond by concentration simultaneously; By blower fan, air is sent into oxidation pond; Finally add sulfuric acid and regulate pH value to be 3 ~ 4, carry out triphase catalytic oxidation reaction, wherein catalyst activity component is ferrous sulfate, and temperature of reaction is 50 DEG C ~ 60 DEG C, and the reaction times is 4h ~ 8h; After having reacted, the waste water after process is entered wastewater equalization pond, and adds flocculation agent, then filter and remove suspended substances precipitation, obtains the waste water handled well.
Aforesaid method has brought new impurity into liquid waste disposal, also needs to expend sulfuric acid, hydrogen peroxide etc. simultaneously, adds cost, and the suspended substance comparison of ingredients simultaneously generated is complicated, needs to process recovery further.In order to make recovery process simpler, reduce cost recovery, publication number is the application for a patent for invention file of 101139148A, disclose a kind for the treatment of process and special extractor thereof of sebacic acid factory effluent: adopt ricinolic acid to extract as extraction agent and prohibit row's thing, and by special multi-stage solvent extraction device cyclical operation, realization taboo row thing is separated 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 of cooling, the sebacic acid of crystallization to return in sebacic acid preparation technology purifying again, supernatant liquid in cooling pool (1) enters the first pH value equalizing tank (2), the pH value regulating 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, water-oil phase is fully contacted, extraction tower (6) top is discharged containing phenol ricinolic acid, enter in the first water-and-oil separator (7), the cleavage step of returning containing phenol ricinolic acid in sebacic acid preparation technology that first water-and-oil separator (7) top is discharged, the organism that first water-and-oil separator (7) bottom is discharged goes back to extraction tower (6) top, reflux ratio is 1: 1 to 1: 8, waste water after dephenolize escapes 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 second pH value equalizing tank (9) containing nitre waste water, the pH value regulating 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 after the centrifugation of whizzer (21), dry in moisture eliminator (22), thus obtain solid sodium sulfate powder.
But aforesaid method, substantially being adopt extraction agent to extract phenol, needing to add extraction agent, to bringing new impurity in waste water, the pervaporation simultaneously adopted 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 recycling device method high cost of existing Preparation of Sebacic Acid From Castor Oil generation and the problems such as new impurity can be brought 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 solving the 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. adjust ph: add sodium hydroxide in waste water, adjust ph is 8-13, and this step can be carried out in various large container, 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 fatty acid impurities; Described waste water after adding sodium hydroxide, lipid acid generation saponification reaction.
B. lipid acid purification: by the waste water through a step process through air-float method or the process of micro-filtration method, the vesicle of waste liquid height of formation dispersion, form water-gas-particle three-phase mixed system, sodium soap to be attached on bubble and to float to the water surface and forms scum layer, then scum layer is scraped off, namely remove fatty acid impurities, 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 with the temperature of 50-120 DEG C under carry out evaporating and crystallization treatment, obtain Sodium sulfate anhydrous.min(99) slurries, secondary steam and water of condensation.Containing phenol in secondary steam.
D. Sodium sulfate anhydrous.min(99) slurries solid-liquid separation: the Sodium sulfate anhydrous.min(99) slurries obtained through step c are carried out solid-liquid separation process, this solid-liquid separation process can adopt the devices such as whizzer to carry out, obtain the solid of separation and the liquid be separated, then isolated liquid is imported in the function of mechanical steam recompression evaporation and crystallization system in step c by pump;
E. secondary steam is except phenol purification: passed in steam purifier by the secondary steam obtained through step c and carry out purifying treatment, be added with sodium hydroxide solution in described steam purifier, obtain the secondary steam of sodium phenylate solution and purification;
F. secondary steam compression: the secondary steam of the purification obtained through step e process is carried out processed compressed, then passes 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, become water of condensation after steam source and wastewater heat exchange, and waste water is that secondary steam, simultaneously waste water are concentrated by portions turn during thermal evaporation; 2. secondary steam first compresses using the temperature improving steam, pressure then as the thermal source of evaporation through vapour compressor except after phenol purification again.Owing to containing a large amount of phenol in secondary steam, for the water quality and minimizing that ensure water of condensation are carried out except phenol process to water of condensation again, so must carry out except phenol purification to secondary steam, sodium hydroxide and phenol generation chemical reaction is utilized to generate the principle of sodium phenylate, with the scavenging agent of sodium hydroxide as phenol in secondary steam, reclaim sodium phenylate; 3. waste water is constantly by evaporation concentration, when the sodium sulfate concentration in waste water exceedes its saturation concentration at that time at temperature, the continuous crystallization of sodium sulfate forms particulate state sodium sulfate (Sodium sulfate anhydrous.min(99)) crystal not of uniform size with growing up, and crystal forms Sodium sulfate anhydrous.min(99) slurry in the bottom enrichment of crystallizer under the effect of deadweight.
G. repeating step c-f at least one times, then collects sodium phenylate solution, the solid be separated that water of condensation obtains with Step d.Carry out this step, after concentrated Sodium sulfate anhydrous.min(99) slurries centrifugation, mother liquor is continued to return in evaporative crystallizer, then circulation is realized along with the waste liquid in evaporative crystallizer imports to heating chamber top by concentrated solution recycle pump, and realize heat exchange in period through during heating chamber, carry out condensing crystal further by thermal evaporation, circulation repeatedly makes the sulfate crystal in waste water separate out; The phenol contained in secondary steam, by generating sodium phenylate after sodium hydroxide solution, makes the overwhelming majority of the phenol in secondary steam be absorbed by sodium hydroxide solution after steam repeatedly circulates
In the present invention, preferably, the solid of the separation of g collection step is carried out drying treatment, obtained dry Sodium sulfate anhydrous.min(99), then packs;
In the present invention, preferably, the sodium phenylate solution of g collection step is reclaimed.
In the present invention, preferably, the water of condensation described step c obtained carries out heat exchange by interchanger, then by the condensation water collection after heat exchange with the waste water produced by Preparation of Sebacic Acid From Castor Oil.
A device for the waste water recycling device 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 room and is connected with its upper opening, described heating chamber is provided with the first opening for feed, first discharge port, secondary heat source entrance and condensation-water drain, be provided with slurry outlet and whizzer mother liquor reflux mouth bottom described evaporative crystallization room, the sidewall of described evaporative crystallization room is provided with the second opening for feed, secondary steam exports, and described slurry outlet is connected with whizzer by pipeline, and described whizzer is provided with slurry inlet, whizzer mother liquor outlet and solids exit mouth, described whizzer mother liquor outlet by pipeline successively with whizzer mother liquor reflux pump, whizzer mother liquor reflux mouth bottom evaporative crystallization room connects, and described concentrated solution recycle pump carries pump outlet with waste material respectively by threeway and/or by-pass line, the first opening for feed on heating chamber, second opening for feed of evaporative crystallization room 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 solids exit mouth 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, described pipeline is equipped with valve.
The invention provides wastewater recovery processing technique and the device of the generation of a kind of Preparation of Sebacic Acid From Castor Oil, 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 circulation is realized along with the waste liquid in evaporative crystallizer imports to heating chamber top by concentrated solution recycle pump, and realize heat exchange in period through during heating chamber, carry out condensing crystal further by thermal evaporation, circulation repeatedly makes the sulfate crystal in waste water separate out; The phenol contained in secondary steam, by generating sodium phenylate after sodium hydroxide solution, makes the overwhelming majority of the phenol in secondary steam be absorbed by sodium hydroxide solution after steam repeatedly circulates; Then, the steam of purification by vapour compressor compression, heat up after pass into heat exchanger in heating chamber, the water of condensation that steam exothermic condensation is formed can Collection utilization; Then collect reuse Sodium sulfate anhydrous.min(99), sodium phenylate solution and water of condensation, achieve the resource utilization reuse of waste water and the zero release of poisonous and harmful waste water, not only reduce production cost but also protect environment.
By the evaporative crystallization Treatment for Reuse of function of mechanical steam recompression system to waste water, do not bring the interpolation of other compositions in existing recovery process into, decrease processing step and extraction cost; Mechanical vapor recompression technology is adopted to concentrate waste liquid in the present invention, only need use relatively few energy, the mechanical energy of the compressor impeller namely in compressing hot pump situation, energy to be added in technique heating medium and to enter continuous circulation, significantly reduces energy consumption needed for recovery process; In addition, the recycling and processing device in the present invention, equipment is simpler compared with legacy equipment, easy to operate.
Below in conjunction with the drawings and the specific embodiments, the present invention is described in further detail.
Accompanying drawing explanation
The embodiment of the present invention is illustrated further 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 illustrates: 1, PH equalizing tank; 2, lipid acid cleaner; 21, waste liquid transferpump; 3, evaporative crystallizer 3; 31, concentrated solution recycle pump; 32, evaporative crystallization room; 321, the second opening for feed; 322, slurry outlet; 323, whizzer mother liquor reflux mouth; 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
To the waste water reclamation that 1 ton of Preparation of Sebacic Acid From Castor Oil produces, through detecting, contriver records sodium sulfate 150g/L in this waste water, phenol 2000mg/L, fatty acid impurities 5000mg/L, COD8500mg/L, pH value 2.8.For this batch of waste liquid, adopt as lower device recycles:
A device for the waste water recycling device 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 room 32 and is connected with its upper opening, described heating chamber 33 is provided with the first opening for feed 333, first discharge port 334, secondary heat source entrance 331 and condensation-water drain 332, be provided with slurry outlet 322 and whizzer mother liquor reflux mouth 323 bottom described evaporative crystallization room 32, the sidewall of described evaporative crystallization room 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 inlet, whizzer mother liquor outlet and solids exit mouth, described whizzer mother liquor outlet by pipeline successively with whizzer mother liquor reflux pump 41, whizzer mother liquor reflux mouth 323 bottom evaporative crystallization room 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, second opening for feed 321 of evaporative crystallization room 32 sidewall connects, described secondary steam outlet 324 by pipeline successively with vacuum pump 10, steam purifier 6, vapour compressor 7 is connected with secondary heat source entrance 321.
The solids exit mouth 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.Described pipeline is equipped with valve.
Recycling step is as follows:
A. adjust ph: waste water is added in pH regulator pond 1, then add sodium hydroxide in waste water, adjust ph 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 fatty acid impurities;
B. lipid acid purification: the waste water through b step process to be added by pipeline lipid acid cleaner 2 through air-float method process from the discharge port in pH regulator pond 1, scrapes off scum layer;
C. evaporative crystallization: the waste water through step c process is added in the evaporative crystallization room 32 of the evaporative crystallizer 3 in function of mechanical steam recompression system by waste material transferpump 21, then to carry out at the temperature of 50-120 DEG C evaporating and crystallization treatment, Sodium sulfate anhydrous.min(99) slurries, secondary steam and water of condensation is obtained;
D. Sodium sulfate anhydrous.min(99) slurries solid-liquid separation: the Sodium sulfate anhydrous.min(99) slurries obtained through step c are carried out solid-liquid separation process by whizzer 4, obtains the solid of separation and the liquid be separated, is then pumped into by isolated liquid in the function of mechanical steam recompression system in step c;
E. secondary steam is except phenol purification: the secondary steam obtained through step c is passed into vacuum pump 10 and be transported in steam purifier 6 and carry out purifying treatment, be added with sodium hydroxide solution, obtain the secondary steam of sodium phenylate solution and purification in described steam purifier 6;
F. secondary steam compression: the secondary steam of the purification obtained through step e process is carried out processed compressed by vapour compressor 7, then passes in function of mechanical steam recompression system;
G. repeating step c-f, then collects sodium phenylate solution, the solid be separated that water of condensation obtains with Step d, and is then carried out dryly obtaining dry Sodium sulfate anhydrous.min(99), then through packaging acquisition product through dry packing machine 5 by the solid of the separation of collecting; Sodium phenylate solution sodium phenylate solution recovery pump 8 is collected; By water of condensation by recycling condensing water pump 9 recycling.
Detect the Sodium sulfate anhydrous.min(99) after reclaiming, sodium sulphate content is greater than 98.5%, is qualified industry II grade of Sodium sulfate anhydrous.min(99); In water of condensation, the concentration of phenol is 0.05mg/L after testing, and decontamination effect improving is excellent, and water of condensation is gradable to be back in production.Can find out, after the present invention program's process, the separated and reuse of the substance fatty acid in waste liquid, phenol and sodium sulfate, Treatment for Reuse is respond well, substantially achieves 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, change and the replacement of any unsubstantiality that those skilled in the art does on basis of the present invention all belong to the present invention's scope required for protection.
Claims (4)
1. a wastewater recovery processing technique for Preparation of Sebacic Acid From Castor Oil generation, is characterized in that comprising the steps:
A. adjust ph: add sodium hydroxide in waste water, adjust ph 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 fatty acid impurities;
B. lipid acid purification: by the waste water through a step process through air-float method or the process of micro-filtration method, except removing dross;
C. evaporative crystallization: by the waste water through b step process in function of mechanical steam recompression system with the temperature of 50-120 DEG C under carry out evaporating and crystallization treatment, obtain Sodium sulfate anhydrous.min(99) slurries, secondary steam and water of condensation;
D. Sodium sulfate anhydrous.min(99) slurries solid-liquid separation: the Sodium sulfate anhydrous.min(99) slurries obtained through step c are carried out solid-liquid separation process, obtains the solid of separation and the liquid be separated, and then imports in the function of mechanical steam recompression evaporation and crystallization system in step c by isolated liquid by pump;
E. secondary steam is except phenol purification: passed in steam purifier by the secondary steam obtained through step c and carry out purifying treatment, be added with sodium hydroxide solution in described steam purifier, obtain the secondary steam of sodium phenylate solution and purification;
F. secondary steam compression: the secondary steam of the purification obtained through step e process is carried out processed compressed, then passes in function of mechanical steam recompression system;
G. repeating step c-f at least one times, then collects sodium phenylate solution, the solid be separated that water of condensation obtains with Step d;
The device that the wastewater recovery processing technique that described Preparation of Sebacic Acid From Castor Oil produces adopts 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 room and is connected with its upper opening, described heating chamber is provided with the first opening for feed, first discharge port, secondary heat source entrance and condensation-water drain, be provided with slurry outlet and whizzer mother liquor reflux mouth bottom described evaporative crystallization room, the sidewall of described evaporative crystallization room is provided with the second opening for feed, secondary steam exports, and described slurry outlet is connected with whizzer by pipeline, and described whizzer is provided with slurry inlet, whizzer mother liquor outlet and solids exit mouth, described whizzer mother liquor outlet by pipeline successively with whizzer mother liquor reflux pump, whizzer mother liquor reflux mouth bottom evaporative crystallization room connects, and described concentrated solution recycle pump carries pump outlet with waste material respectively by three-way pipeline and/or by-pass line, the first opening for feed on heating chamber, second opening for feed of evaporative crystallization room 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.
2. the wastewater recovery processing technique of Preparation of Sebacic Acid From Castor Oil generation according to claim 1, is characterized in that: the solid of the separation of g collection step is carried out drying treatment, and obtained dry Sodium sulfate anhydrous.min(99), then packs.
3. the wastewater recovery processing technique of Preparation of Sebacic Acid From Castor Oil generation according to claim 1, is characterized in that: reclaimed by the sodium phenylate solution of g collection step.
4. the wastewater recovery processing technique of Preparation of Sebacic Acid From Castor Oil generation according to claim 1, it is characterized in that: the water of condensation described step c obtained carries out heat exchange by interchanger, then by the condensation water collection after heat exchange with the waste water produced by Preparation of Sebacic Acid From Castor Oil.
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| CN107128988B (en) * | 2017-04-13 | 2019-08-06 | 江苏瑞升华能源科技有限公司 | A kind of waste water crystal system containing sodium sulphate |
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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 |
| CN109694111B (en) * | 2019-01-31 | 2022-08-26 | 合众思(北京)环境工程有限公司 | Flash evaporation salt separation process for high COD (chemical oxygen demand) and nitrate mother liquor |
| CN111137965A (en) * | 2019-12-31 | 2020-05-12 | 河北中科同创科技发展有限公司 | Method for treating phenol-free wastewater generated in sebacic acid production process by microwave pyrolysis method |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6071409A (en) * | 1998-07-07 | 2000-06-06 | Abb Lummus Global Inc. | Phenolic wastewater treatment with ethers for removal and recovery of phenolics |
| CN1450006A (en) * | 2002-04-05 | 2003-10-22 | 山东海化天合有机化工有限公司 | Treatment of phenol containing decanedioic acid waste water by extractive distillation |
| CN201305469Y (en) * | 2008-12-11 | 2009-09-09 | 江苏和亿昌环保工程科技有限公司 | A device for extracting desulfurated byproduct ammonium sulphate |
| CN201864580U (en) * | 2010-10-29 | 2011-06-15 | 江苏瑞普膜技术有限公司 | Device producing thenardite by sodium sulfate decahydrate |
| CN102311195A (en) * | 2011-06-24 | 2012-01-11 | 扬州大学 | Recycling utilization and processing method for wastewater generated in sebacic acid production process |
| CN102745755A (en) * | 2011-10-25 | 2012-10-24 | 河北凯徳生物材料有限公司 | Process for recovering sodium sulfate crystal in sebacic acid production |
| CN103145153A (en) * | 2013-04-11 | 2013-06-12 | 南风化工集团股份有限公司 | Application of MVR (Mechanical Vapor Recompression) crystallization evaporator to industrialized production of anhydrous sodium sulphate |
| CN203754551U (en) * | 2014-01-28 | 2014-08-06 | 广州新普利节能环保科技有限公司 | Device for recycling and treating waste water produced during preparation of decanedioic acid by utilizing castor oil |
-
2014
- 2014-01-28 CN CN201410042559.0A patent/CN103787542B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6071409A (en) * | 1998-07-07 | 2000-06-06 | Abb Lummus Global Inc. | Phenolic wastewater treatment with ethers for removal and recovery of phenolics |
| CN1450006A (en) * | 2002-04-05 | 2003-10-22 | 山东海化天合有机化工有限公司 | Treatment of phenol containing decanedioic acid waste water by extractive distillation |
| CN201305469Y (en) * | 2008-12-11 | 2009-09-09 | 江苏和亿昌环保工程科技有限公司 | A device for extracting desulfurated byproduct ammonium sulphate |
| CN201864580U (en) * | 2010-10-29 | 2011-06-15 | 江苏瑞普膜技术有限公司 | Device producing thenardite by sodium sulfate decahydrate |
| CN102311195A (en) * | 2011-06-24 | 2012-01-11 | 扬州大学 | Recycling utilization and processing method for wastewater generated in sebacic acid production process |
| CN102745755A (en) * | 2011-10-25 | 2012-10-24 | 河北凯徳生物材料有限公司 | Process for recovering sodium sulfate crystal in sebacic acid production |
| CN103145153A (en) * | 2013-04-11 | 2013-06-12 | 南风化工集团股份有限公司 | Application of MVR (Mechanical Vapor Recompression) crystallization evaporator to industrialized production of anhydrous sodium sulphate |
| CN203754551U (en) * | 2014-01-28 | 2014-08-06 | 广州新普利节能环保科技有限公司 | Device for recycling and treating waste water produced during preparation of decanedioic acid by utilizing castor oil |
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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 |