CN101781010B - Novel treatment process for cyclic utilization of high-concentration sodium cyanide-containing waste water - Google Patents
Novel treatment process for cyclic utilization of high-concentration sodium cyanide-containing waste water Download PDFInfo
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- CN101781010B CN101781010B CN2010101253697A CN201010125369A CN101781010B CN 101781010 B CN101781010 B CN 101781010B CN 2010101253697 A CN2010101253697 A CN 2010101253697A CN 201010125369 A CN201010125369 A CN 201010125369A CN 101781010 B CN101781010 B CN 101781010B
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- sodium cyanide
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- 239000002351 wastewater Substances 0.000 title claims abstract description 66
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 28
- 125000004122 cyclic group Chemical group 0.000 title abstract 2
- MNWBNISUBARLIT-UHFFFAOYSA-N sodium cyanide Chemical compound [Na+].N#[C-] MNWBNISUBARLIT-UHFFFAOYSA-N 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- IRUJZVNXZWPBMU-UHFFFAOYSA-N cartap Chemical compound NC(=O)SCC(N(C)C)CSC(N)=O IRUJZVNXZWPBMU-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000009835 boiling Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000010521 absorption reaction Methods 0.000 claims abstract description 18
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims abstract description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000007255 decyanation reaction Methods 0.000 abstract 1
- 150000007522 mineralic acids Chemical class 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 29
- 235000010265 sodium sulphite Nutrition 0.000 description 14
- 238000011084 recovery Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- NMOJAXCSURVGEY-UHFFFAOYSA-N N#CC#N.[S] Chemical compound N#CC#N.[S] NMOJAXCSURVGEY-UHFFFAOYSA-N 0.000 description 1
- 230000003851 biochemical process Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
The invention relates to a novel treatment process for the cyclic utilization of high-concentration sodium cyanide-containing waste water generated in the cartap synthetic process. The novel treatment process comprises the following steps: 1) putting the high-concentration sodium cyanide-containing waste water generated in the cartap synthetic cyanidation section in a closed reactor, vacuum-pumping, slowly dripping 20-60% of inorganic acid, and adjusting the pH value to 4.0-10.0; 2) heating the high-concentration sodium cyanide-containing waste water of which the pH value is adjusted to the boiling point in the vacuum state to release CN- in the form of HCN, wherein the released HCN is absorbed by the prepared 30-35% of sodium hydroxide solution in the reactor; and 3) stopping heating when the concentration of NaCN in the waste water is less than or equal to 30mg/L, and repeatedly and circularly absorbing the HCN released from the cyanide-containing waste water with the sodium hydroxide absorption liquid, wherein the absorption liquid can be used as the cartap for the synthetic cyanidation section when the weight percentage of the NaCN in the absorption liquid is 25-30%, and the residue liquid is directly discharged after the decyanation and biochemical treatment. The invention solves the problem that the high-concentration sodium cyanide-containing waste water is difficult to treat, and achieves the purpose of energy saving and emission reduction.
Description
Technical field
The invention belongs to environmental protection and resource recycling field, be specifically related to the high-concentration sodium cyanide-containing waste water recycle New Process for Treatment that produces in a kind of cartap building-up process.
Background technology
Clam worm poison derivative pesticide is the bionical sterilant of a kind of efficient, low toxicity, wide spectrum, and cartap be use the most extensively in these series product, more efficient, the kind that has more broad spectrum.The earliest by Japan's military field invention and commercialization.Domestic have many research units to research and develop since six the seventies, all the time the progress of achieving no breakthrough property.Just confirm synthesis technique basically up to last century end.Through nearly ten years continue to optimize, reach advanced world standards at present.From the production technique of present domestic cartap, most enterprises all be adopt the desinsection list or disosultap in solvent, obtains sulphur cyanogen thing with sodium cyanide after hydrolysis, precipitation, separate, drying obtains product.This process recovery ratio is high, quality better.Part enterprise adopts muriate or sulfonated liquid method to produce cartap, but its yield is low, product is unstable, and bag, variable color are prone to rise.
Adopt desinsection list or disosultap and sodium cyanide production technique in solvent; Will produce a large amount of high-concentration sodium cyanide-containing waste waters in cyaniding workshop section; After reclaiming, sodium cyanide wherein can be applied in the synthetic cyaniding workshop section of cartap again; So not only make in the high cyanide containing wastewater cyanogen root obtain handling, but also realized resource circulation utilization, reached the energy-saving and emission-reduction purpose.Do not relate to the cyanide wastewater treatment process among the patent of invention 98111505.5 cartap preparing methods.Its technology is advocated on recycling economy and the energy-saving and emission-reduction policy at present and had wretched insufficiency: 1. energy consumption is big.Original cyanide wastewater is to remove cyanogen through high-temperature high-pressure hydrolysis, needs a large amount of thermal source and high-tension apparatus.2. the wasting of resources.In order to improve desinsection list or disosultap transformation efficiency, must add excessive sodium cyanide in cyaniding workshop section, so the cyanogen root is dense in the waste water, generally in 4000mg/L～11OO0mg/L scope.Directly broken cyanide is not handled if do not take recycle and reuse, so not only wastes resource but also treatment effect and is difficult to reach discharging standards.3. contaminate environment.The cyanide wastewater of high density is difficult to handle discharging standards with biochemical process, and its discharging has caused environmental pollution.Patent CN101318630A and patent CN101318671A only recycle S-WAT in the high cyanide containing wastewater of cartap building-up process generation and report, do not report and there is patent that the high cyanide containing wastewater recycle of the synthetic generation of cartap is handled at present.
Summary of the invention
The objective of the invention is to improve and innovate, the high-concentration sodium cyanide-containing waste water recycle New Process for Treatment of cyaniding workshop section generation in a kind of desinsection list or disosultap and the Sodium Cyanide Production cartap technology is provided to shortcoming that exists in the background technology and problem.
Technology of the present invention may further comprise the steps:
1) high-concentration sodium cyanide-containing waste water that the synthetic cyaniding workshop section of cartap is produced places closed reactor, vacuumizes again, slowly drips the mineral acid of 20-60% then, and the adjustment pH value is to 4.0-10.0;
The high-concentration sodium cyanide-containing waste water that 2) will mix up pH value is heated to boiling under vacuum state, make CN
-Form with HCN discharges, and discharges HCN and absorbed by the sodium hydroxide solution of ready 30-35% in the reactor drum;
3) when NaCN concentration in the waste water≤30mg/L, stop heating; The sodium hydroxide absorption liquid repeats repeatedly to circulate again and absorbs the HCN that sodium cyanide-containing waste water discharges; When NaCN quality percentage composition is 25-30% in absorption liquid; Can this absorption liquid be used directly discharging after residual solution process broken cyanide and the biochemical treatment as the synthetic cyaniding workshop section of cartap.
Described mineral acid of the present invention is a phosphoric acid, perhaps phosphorous acid, perhaps nitric acid, perhaps sulfuric acid.
Vacuum tightness of the present invention is 0.02-0.09Mpa, and optimal vacuum pressure is 0.09Mpa.
Best pH value of the present invention is 6.5-7.5.
Heating temperature is 30-70 ℃ under the vacuum state of the present invention, and optimum heating temperature is 40-50 ℃.
The reacting by heating time is 30-70min under the vacuum state of the present invention, and optimum reacting time is 40-50min.
CN in the cyanide wastewater of the present invention
-Concentration is 4000mg/L-11000mg/L.
Of the present invention being recovered utilized and is applied to that NaCN quality percentage composition is 25-30% in the NaCN absorption liquid of the synthetic cyaniding workshop section of cartap.
NaCN concentration≤30mg/L in the cyanide wastewater after the recycle of the present invention.
Under the processing condition of the present invention, the NaCN recovery utilization rate is 94.8-99.3%.
NaCN concentration≤30mg/L after the art breading of the present invention, remaining waste water NaCN concentration≤0.5mg/L after company's treatment center of sewage broken cyanide and biochemical treatment reaches national grade one discharge standard.
The present invention makes NaCN remove rate up to 99.98%; The NaCN cyclic utilization rate is up to more than 94.8%; And full cycle is utilized, and treatment process process energy consumption is low, the recovery is high, NaCN removes rate height, pollution-free; Thoroughly solved the unmanageable problem of high-concentration sodium cyanide-containing waste water, and, reached the purpose of energy-saving and emission-reduction through recycle NaCN.
Embodiment
Embodiment 1:
(its NaCN concentration is 8004.1mg/L to the high density that the synthetic cyaniding workshop section of cartap is produced, Na
2SO
3Concentration is 120.3g/L) sodium cyanide-containing waste water 3000mL places in the encloses container, and the open vacuum pump vacuumizes.When vacuum tightness was 0.07Mpa, it was the pH value to 5.0 that 50% phosphoric acid is transferred sodium cyanide-containing waste water that beginning slowly drips the quality percentage composition.40 ℃ of heating in water bath make sodium cyanide-containing waste water boiling, CN in boiling process
-Discharge and be that 35% 500mL sodium hydroxide solution absorbs with the form of HCN by massfraction.Stop heating behind the sodium cyanide-containing waste water boiling 40min, stop to vacuumize after 5min.Cooling is after measure, and NaCN concentration is that 46679.9mg/L, concentration of sodium sulfite are 6.4281g/L in the absorption liquid; NaCN concentration is that 27.9mg/L, concentration of sodium sulfite are 119.2g/L in the waste water residual solution.The NaCN recovery utilization rate is 97.2%.
Embodiment 2:
(its NaCN concentration is 8011.4mg/L to the high density that the synthetic cyaniding workshop section of cartap is produced, Na
2SO
3Concentration is 122.7g/L) sodium cyanide-containing waste water 3000mL places in the encloses container, and the open vacuum pump vacuumizes.When vacuum tightness was 0.09Mpa, it was the pH value to 5.5 that 50% phosphoric acid is transferred sodium cyanide-containing waste water that beginning slowly drips the quality percentage composition.40 ℃ of heating in water bath make sodium cyanide-containing waste water boiling, CN in boiling process
-Discharge and be that 35% 500mL sodium hydroxide solution absorbs with the form of HCN by massfraction.Stop heating behind the sodium cyanide-containing waste water boiling 40min, stop to vacuumize after 5min.Cooling is after measure, and NaCN concentration is that 47731.9mg/L, concentration of sodium sulfite are 6.5368g/L in the absorption liquid; NaCN concentration is that 20.1mg/L, concentration of sodium sulfite are 121.6g/L in the waste water residual solution.The NaCN recovery utilization rate is 99.2%.
Embodiment 3:
(its NaCN concentration is 8007.5mg/L mg/L to the high density that the synthetic cyaniding workshop section of cartap is produced, Na
2SO
3Concentration is 119.0g/L) sodium cyanide-containing waste water 3000mL places in the encloses container, and the open vacuum pump vacuumizes.When vacuum tightness was 0.09Mpa, it was the pH value to 4.0 that 50% phosphoric acid is transferred cyanide wastewater that beginning slowly drips the quality percentage composition.40 ℃ of heating in water bath make sodium cyanide-containing waste water boiling, CN in boiling process
-Discharge and be that 35% 500mL sodium hydroxide solution absorbs with the form of HCN by massfraction.Stop heating behind the sodium cyanide-containing waste water boiling 40min, stop to vacuumize after 5min.Cooling is after measure, and NaCN concentration is that 47708.6mg/L, concentration of sodium sulfite are 9.2184g/L in the absorption liquid; NaCN concentration is that 25.2mg/L, concentration of sodium sulfite are 117.5g/L in the waste water residual solution.CN
-Recovery utilization rate is 99.3%.
Embodiment 4:
(its NaCN concentration is 8000.6mg/L to the high density that the synthetic cyaniding workshop section of cartap is produced, Na
2SO
3Concentration is 118.4g/L) sodium cyanide-containing waste water 3000mL places in the encloses container, and the open vacuum pump vacuumizes.When vacuum tightness was 0.09Mpa, it was the pH value to 7.0 that 50% phosphoric acid is transferred sodium cyanide-containing waste water that beginning slowly drips the quality percentage composition.40 ℃ of heating in water bath make sodium cyanide-containing waste water boiling, CN in boiling process
-Discharge and be that 35% 500mL sodium hydroxide solution absorbs with the form of HCN by massfraction.Stop heating behind the sodium cyanide-containing waste water boiling 40min, stop to vacuumize after 5min.Cooling is after measure, and NaCN concentration is that 47667.6mg/L, concentration of sodium sulfite are 0.9613g/L in the absorption liquid; NaCN concentration is that 13.9mg/L, concentration of sodium sulfite are 118.2g/L in the waste water residual solution.CN
-Recovery utilization rate is 99.3%.
Embodiment 5:
(its NaCN concentration is 8010.8mg/L to the high density that the synthetic cyaniding workshop section of cartap is produced, Na
2SO
3Concentration is 119.3g/L) sodium cyanide-containing waste water 3000mL places in the encloses container, and the open vacuum pump vacuumizes.When vacuum tightness was 0.09Mpa, it was the pH value to 8.5 that 50% phosphoric acid is transferred sodium cyanide-containing waste water that beginning slowly drips the quality percentage composition.40 ℃ of heating in water bath make sodium cyanide-containing waste water boiling, CN in boiling process
-Discharge and be that 35% 500mL sodium hydroxide solution absorbs with the form of HCN by massfraction.Stop heating behind the sodium cyanide-containing waste water boiling 40min, stop to vacuumize after 5min.Cooling is after measure, and NaCN concentration is that 47151.6mg/L, concentration of sodium sulfite are 0.7216g/L in the absorption liquid; NaCN concentration is that 23.6mg/L, concentration of sodium sulfite are 119.2g/L in the waste water residual solution.CN
-Recovery utilization rate is 98.1%.
Embodiment 6:
(its NaCN concentration is 8008.3mg/L to the high density that the synthetic cyaniding workshop section of cartap is produced, Na
2SO
3Concentration is 119.7g/L) sodium cyanide-containing waste water 3000mL places in the encloses container, and the open vacuum pump vacuumizes.When vacuum tightness was 0.09Mpa, it was the pH value to 9.0 that 50% phosphoric acid is transferred sodium cyanide-containing waste water that beginning slowly drips the quality percentage composition.40 ℃ of heating in water bath make sodium cyanide-containing waste water boiling, CN in boiling process
-Discharge and be that 35% 500mL sodium hydroxide solution absorbs with the form of HCN by massfraction.Stop heating behind the sodium cyanide-containing waste water boiling 40min, stop to vacuumize after 5min.Cooling is after measure, and NaCN concentration is that 45551.2mg/L, concentration of sodium sulfite are 0.3006g/L in the absorption liquid; NaCN concentration is that 15.8mg/L, concentration of sodium sulfite are 119.6g/L in the waste water residual solution.The NaCN recovery utilization rate is 94.8%.
Embodiment 7:
(its NaCN concentration is 8000.1mg/L to the high density that the synthetic cyaniding workshop section of cartap is produced, Na
2SO
3Concentration is 115.5g/L) sodium cyanide-containing waste water 3000mL places in the encloses container, and the open vacuum pump vacuumizes.When vacuum tightness was 0.09Mpa, it was the pH value to 7.5 that 50% phosphorous acid is transferred sodium cyanide-containing waste water that beginning slowly drips the quality percentage composition.40 ℃ of heating in water bath make sodium cyanide-containing waste water boiling, CN in boiling process
-Discharge and be that 35% 500mL sodium hydroxide solution absorbs with the form of HCN by massfraction.Stop heating behind the sodium cyanide-containing waste water boiling 40min, stop to vacuumize after 5min.Cooling is after measure, and NaCN concentration is that 47616.6mg/L, concentration of sodium sulfite are 0.9418g/L in the absorption liquid; NaCN concentration is that 14.4mg/L, concentration of sodium sulfite are 115.3g/L in the waste water residual solution.The NaCN recovery utilization rate is 99.2%.
Embodiment of the present invention only is the description that preferred implementation of the present invention is carried out; Be not that design of the present invention and scope are limited; Under the prerequisite that does not break away from design philosophy of the present invention, engineering technical personnel make technical scheme of the present invention in this area various modification and improvement all should fall into protection scope of the present invention; The technology contents that the present invention asks for protection all is documented in claims.
Claims (1)
1. high-concentration sodium cyanide-containing waste water recycle treatment process is characterized in that may further comprise the steps:
1) high-concentration sodium cyanide-containing waste water that the synthetic cyaniding workshop section of cartap is produced places closed reactor, vacuumizes again, slowly drips the mineral acid of 20-60% then, and adjustment pH value is to 4.0-10.0;
The high-concentration sodium cyanide-containing waste water that 2) will mix up the pH value is heated to boiling under vacuum state, make CN
-Form with HCN discharges, and discharges HCN and absorbed by the sodium hydroxide solution of ready 30-35% in the reactor drum;
3) when NaCN concentration in the waste water≤30mg/L, stop heating; The sodium hydroxide absorption liquid repeats repeatedly to circulate again and absorbs the HCN that sodium cyanide-containing waste water discharges; When NaCN quality percentage composition is 25-30% in absorption liquid; Can this absorption liquid be used directly discharging after residual solution process broken cyanide and the biochemical treatment as the synthetic cyaniding workshop section of cartap; Wherein:
Described mineral acid is a phosphoric acid, perhaps phosphorous acid, perhaps nitric acid, perhaps sulfuric acid;
Vacuum tightness is 0.02-0.09Mpa, and Heating temperature is 30-70 ℃ under the vacuum state, and the reacting by heating time is 30-70min under the vacuum state;
CN in the described sodium cyanide-containing waste water
-Concentration is 4000mg/L-11000mg/L;
Be recovered and utilize and be applied to that NaCN quality percentage composition is 25-30% in the NaCN absorption liquid of the synthetic cyaniding workshop section of cartap.
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| CN2010101253697A CN101781010B (en) | 2010-03-17 | 2010-03-17 | Novel treatment process for cyclic utilization of high-concentration sodium cyanide-containing waste water |
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|---|---|---|---|
| CN2010101253697A CN101781010B (en) | 2010-03-17 | 2010-03-17 | Novel treatment process for cyclic utilization of high-concentration sodium cyanide-containing waste water |
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| CN110470789B (en) * | 2019-08-26 | 2022-07-05 | 四川达兴能源股份有限公司 | Method for determining hydrogen cyanide in coke oven gas |
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| CN1283568C (en) * | 2003-08-15 | 2006-11-08 | 韩玲萍 | Cyanogen-containing waste water treating method and treating system thereof |
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Application publication date: 20100721 Assignee: Hunan Weimo New Material Co.,Ltd. Assignor: HUNAN GOFAR FINE CHEMICAL TECH. CO.,LTD. Contract record no.: X2023980047358 Denomination of invention: A High Concentration Sodium Cyanide Wastewater Recycling Treatment Process Granted publication date: 20120215 License type: Common License Record date: 20231120 |
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