CN1288101C - Method for treating sawage generated by preparing carbide slag - Google Patents
Method for treating sawage generated by preparing carbide slag Download PDFInfo
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- CN1288101C CN1288101C CN 200510020250 CN200510020250A CN1288101C CN 1288101 C CN1288101 C CN 1288101C CN 200510020250 CN200510020250 CN 200510020250 CN 200510020250 A CN200510020250 A CN 200510020250A CN 1288101 C CN1288101 C CN 1288101C
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Abstract
The present invention discloses a treatment method for waste water generated in the process of preparing acetylene by using calcium carbide. Salt solution with Fe, Zn and Cu is utilized to convert pollutants in the waste water into metallic compound precipitates; then the acidolysis procedure is carried out on the precipitates; and the obtained hydrogen sulphide (H2S) gas and the salt solution with Fe, Zn and Cu are respectively recycled. The salt solution with Fe, Zn and Cu is used for treating the waste water again; the H2S gas is sprinkled and absorbed by using NaOH liquid; the obtained sodium sulfide / sodium hydrosulfide is processed and packaged into products; and elemental sulfur is produced by oxidation. The suspended substances in the water are less than 30 milligrams per liter, the chemical oxygen demand is lower than 100 milligrams per liter, the biochemical oxygen demand is lower than 30 milligrams per liter, and the concentration of the sulfide (measured by S<2->) is lower than 1 milligram per liter after the waste water is treated. Each index achieves the state standard of effluent discharge. Irregular harmful gas is not generated; gases, solids and liquids generated in the treating procedure are reasonably utilized, and no pollutant is discharged. The treatment method obtains obvious economic effects when efficiently treating the pollution.
Description
Technical field
The present invention relates to processing method of industrial waste water, specifically, is the wastewater treatment method that produces in a kind of preparation of ethyne by carbide process.
Background technology
China's preparation of ethyne by carbide is mainly used in the resin industry, and the calcium carbide that wherein only is used to produce PVC just accounts for more than 50% of China's calcium carbide output.Because it is with low cost that the carbide raw material route is produced resin, produce the low 30%-40% of cost of PVC than petroleum cracking, the China's oil inadequate resource, along with oil price soars, the carbide raw material route has bigger cost advantage, and preparation of ethyne by carbide has become the main raw material route of China's vinyl polymerization production of resins.Only be example with polyvinyl chloride resin, the PVC of China 38.44% adopts the carbide acetylene raw material route to produce, and along with Economic development, development space is also very big.But, being used to produce the acetylene gas purity requirement height of resin, the carbide slag pulp-water can not be reused, and a large amount of high-concentration waste waters efflux serious environment pollution.The strictness of western developed country environmental protection policy, oil is supplied with relatively more sufficient, production of resins adopts the petroleum cracking raw material route, do not adopt the carbide acetylene raw material route, market and technical need that acetylene sludge wastewater is handled all do not exist, the research of also not being correlated with, therefore, acetylene sludge wastewater is the distinctive trade effluent of China.The existing calcium carbide output of China reaches more than 700 ten thousand tons, also has the project of nearly 1,000,000 tons of throughput to be in the construction.Preparation of ethyne by carbide per ton will produce the acetylene sludge wastewater more than 10 tons.Chemical oxygen demand (COD), is not effectively administered considerably beyond discharging standards (being lower than 100 mg/litre) so far up to the 700-1200 mg/litre in the waste water.
Usually, resin enterprise acetylene sludge wastewater pollutent index is approximately as follows: PH:13～14; Suspended substance (SS): 40～60 mg/litre; Chemical oxygen demand (COD) (COD
Cr): 600～730 mg/litre; Five-day BOD (BOD
5): 30～40 mg/litre; Sulfide is (with S
2-Meter): 1000～1500 mg/litre (water consumption with calcium carbide per ton changes).In addition, have trace acetylene to be dissolved in the water body, concentration changes with temperature Change.
Acetylene sludge wastewater is not effectively administered, and becomes one of restraining factors of this industry development for a long time.Along with China's water resources is supplied with the outstanding of contradiction, the national environmental protection policy is strict more, and some enterprises face to stop production and administer; Or the limit production scale, can not obtain scale and benefit; Some projects under and awaiting construction press for improvement, otherwise can not put into production.The mature technology that China does not also handle at acetylene sludge wastewater.The waste water of each production of resins enterprise enters waters such as rivers without effective processing, causes huge pollution.Known to a tree name applicant, up to the present, have only two kinds of art breading acetylene sludge wastewaters, the one, the catalyzed oxidation technology; The 2nd, acidifying absorption process technology, these two kinds of treatment technologies all do not obtain promising result.
Catalyzed oxidation is that mechanical oxygen supply of while is with the reducing substances in the oxidation acetylene sludge wastewater to strong oxidizers such as acetylene sludge wastewater adding permanganates.The processing cycle that catalytic oxidation is handled acetylene sludge wastewater generally needs several hrs to tens hour, just can make in the water body chemical oxygen demand (COD) up to standard.Construction investment is big, builds the treatment project of per hour handling 300 tons of acetylene sludge wastewaters, and investment is about 1,500 ten thousand yuan; Since to use strong oxidizers such as permanganate, the working cost height, and processing costs is that 4 yuan (Renminbi)/more than the cubic meter, annual required processing costs is up to 800～10,000,000 yuan.1., treating processes has the hydrogen sulfide uncontrollable discharge, causes topsoil catalyzed oxidation also has following shortcoming:, many unsafe factors lie dormant; 2., manganese belongs to heavy metal, generation heavy metal contamination.
The acidifying absorption process is that handled thing does not have chemical valence to change with the sulfide in the acid displacement waste water.Advantage is: the hydrogen sulfide of generation is collected, recycles, and does not produce heavy metal contamination, can solve the useless vitriolic that produces in the production of resins and use problem, and concentration of treatment is unrestricted substantially.Shortcoming is: the treatment time is long, handles not thoroughly, still has the part pollutent to transfer in the air, and clearance can only reach 90%, can not handle up to standardly, and effect is also unstable; Water ph value after treatment is about 3, also needs acid-base neutralisation to handle; Running cost and treatment project investment are still very big.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of acetylene sludge wastewater integrated conduct method, and this method not only will make the environmental protection index of acetylene sludge wastewater up to standard comprehensively, can be recycled, and the realization resource recycling, thoroughly decontamination has significant environmental benefit; In addition, this method treatment time is short, the efficient height, and construction investment is few, and running cost is low, turns waste into wealth, and has tangible economic benefit.
For realizing above purpose, the present invention mainly solves following key problem in technology:
Chemical oxygen demand (COD) height, sulfide content height are that acetylene sludge wastewater can not reusable reason.As long as remove desulfuration effectively, chemical oxygen demand (COD) just can be up to standard, and acetylene sludge wastewater just can satisfy the production needs of producing acetylene, obtains recycling.
The acetylene sludge wastewater chemical oxygen demand (COD) is very high, mainly is that the reductibility of negative divalent sulfur causes.Sulphur is with negative divalence (S
2-) and calcium ion forms sulfurated lime and calcium polysulfide is dissolved in the water, can not natural subsidence remove, and also should not handle with biological process.
This method for treating sawage generated by preparing carbide slag is to make the pollutent in the acetylene sludge wastewater form precipitation with the divalent sulfur hydrochlorate of iron or zinc or copper or hydrochloride, and liquid-solid phase is separated, and liquid phase is sent acetylene back to and workshop section takes place recycled or discharge; The solid phase precipitation thing is through acidolysis, secondary metal salt and reclaim sulphur, and concrete steps are as follows:
1. reaction tank is gone in wastewater collection, following reaction, take place in the iron of molar equivalents such as adding and sulfides from wastewater or the divalent sulfur hydrochlorate or the hydrochloride of zinc or copper under normal temperature, normal pressure:
In the formula: M is iron or zinc or copper
That is, generate the metallic sulfide of Iron sulfuret or zinc sulphide or cupric sulfide, continue to stir, do not continue to produce up to there being precipitation;
2. will send into the settling tank sedimentation through above-mentioned reacted wastewater, solid-liquid separation, supernatant liquor is sent acetylene generation workshop section back to and is recycled or discharge, and precipitation is sent into closed reactor;
3. add dilute sulphuric acid or hydrochloric acid acid with metallic sulfide (MS) molar equivalent of etc.ing to closed reactor, under normal temperature, normal pressure with precipitate in metallic sulfide following reaction takes place:
That is, generate hydrogen sulfide and ferrous salt or zinc salt or mantoquita, till no longer including the gas generation;
4. with hydrogen sulfide (H
2S) send into gas-holder; The liquid metal salts solution turns back to the metal-salt storage tank, is used for the reaction of above-mentioned steps (1);
5. with hydrogen sulfide (H
2S) be prepared into sulphur or sulfide product.
Described with hydrogen sulfide (H
2S) being prepared into sulphur or sulfide product, is preparation elemental sulfur or sodium sulphite or Sodium sulfhydrate.
The described stirring time length of step (1) is 3～10 minutes, and reaction control condition is that the pH value of water body is 6.5～7.
Described dilute sulphuric acid of step (3) or hydrochloric acid, the control condition of reaction are that the pH value of liquid phase is not less than 2; The concentration 10～70% of described dilute sulphuric acid.
The step of preparation sodium sulphite is: with hydrogen sulfide (H
2S) send into gas absorbing device, and press H
2S: NaOH=1: 2 mole numbers sodium hydroxide solution absorbing hydrogen sulphide (H
2S), generate sodium sulphite (Na
2S), dry packing is a product.
The step of preparation Sodium sulfhydrate is: with hydrogen sulfide (H
2S) send into gas absorbing device, and press H
2S: NaOH=1: 1 mole number sodium hydroxide solution absorbing hydrogen sulphide (H
2S), generate Sodium sulfhydrate (NaHS), dry packing is a product.
The step of preparation elemental sulfur is: with hydrogen sulfide (H
2S) send into airtight oxidation unit, aerating oxygen (O
2) oxidation, generate elemental sulfur (S).
Acetylene sludge wastewater by above-mentioned processing after, all indexs all reach national wastewater discharge standard, do not have the inorganization obnoxious flavour to produce, the gas in the treating processes, solid, liquid phase product all rationally utilize, and do not have pollutant emission, have administered pollution effectively.Following table one is that the acetylene sludge wastewater of Sichuan enterprise adopts the present invention to handle, " the water quality monitoring (WQM) analysis report " provided by environmental monitoring station of China Second Heavy Machinery Group Co, report shows: suspended substance in the water (SS) is lower than 30 mg/litre, chemical oxygen demand (COD) (COD
Cr) be lower than 100 mg/litre, biochemical oxygen demand (BOD) (BOD
5) being lower than 30 mg/litre, sulfide is (with S
2-Meter) concentration is lower than 1 mg/litre.
Table one water quality monitoring (WQM) analysis
| Analysis project | Analytical results (mg/L) | Emission standard (mg/L) | |
| Before the processing | After the processing | ||
| COD cr | 673 | 87 | 100 |
| SS | 54.0 | 23.0 | 60 |
| BOD 5 | 29.5 | 21.0 | 30 |
| S 2- | 1193 | 0.2 | 1.0 |
The method scope of application of the present invention is wide, can handle the acetylene sludge wastewater of any high chemical oxygen demand; Be swift in response thoroughly, the processing cycle is no more than 1 hour.
Adopt method of the present invention, water and handle used main chemical feedstocks and recycle, for production of resins enterprise, solve the useless vitriolic of enterprise simultaneously and used approach, also byproduct---the stock of liquid caustic soda have found new outlet in order to alleviate to produce sodium sulphite or Sodium sulfhydrate.
According to the sewage treatment project that the present invention builds, reduced investment is compared with catalytic oxidation, equal processing power, and investment only 2/3, the construction period is short, and processing costs is low; The chemical oxygen demand (COD) of Sichuan production of resins enterprise acetylene sludge wastewater is that 673 mg/litre, sulfide are 1193 mg/litre, handles with method of the present invention, after the benefit that the recovery resource produces offsets processing costs, can maintain an equal level.
Following table two is seen in the technology of the present invention and prior art, economical effectiveness contrast.
The technology of table two the present invention and prior art, economical effectiveness contrast
| The present invention | Catalytic oxidation | The acidifying absorption process |
| Chemical settling, in the treating processes, substance to be processed does not have valency to change, and is the chemical replacement reaction. | In the treating processes, substance to be processed has valent variation. | With the acid displacement, handled thing does not have chemical valence to change. |
| Reaction is fast, the treatment time short (being no more than 1 hour).Handle thorough, effect stability.Handle up to standard. | Treatment time long (3～13 hours).Handle not thorough, the effect instability.Be difficult for handling up to standard. | Treatment time is long.Handle not thorough, the effect instability.Can not handle up to standard. |
| The sinking agent main component recycles. | Catalyzer once uses, and need constantly add. | Need constantly to add acid. |
| The hydrogen sulfide that the salt removal process produces is collected, recycles. | Treating processes has obnoxious flavour (hydrogen sulfide) to produce, can't reclaim, uncontrollable discharge, unsafe factor lies dormant. | The hydrogen sulfide that treating processes produces is collected, recycles. |
| Do not produce other pollutions | New heavy metal contamination is arranged | Produce acid pollution |
| Can solve the useless vitriolic that produces in the production of resins and use problem. | Can not solve the useless vitriolic that produces in the production of resins and use problem. | Can solve the useless vitriolic that produces in the production of resins and use problem. |
| Concentration of treatment is unrestricted | Be not suitable for the acetylene sludge wastewater of the thousands of mg/litre of chemical oxygen demand (COD) | Concentration of treatment is unrestricted substantially |
| Processing condition are normal temperature and pressure | Processing condition are normal temperature and pressure | Processing condition are condition of negative pressure |
| Processing costs is low | The processing costs height | The handling height |
| The treatment project reduced investment is 2/3 of catalytic oxidation treatment project investment. | The treatment project investment is big | The treatment project investment is big |
Description of drawings
Fig. 1 is the process flow sheet of one embodiment of the present invention
Embodiment
Embodiment one uses the ferrous sulfate sedimentation
Referring to Fig. 1: acetylene sludge wastewater is collected into water collecting basin, sends into equalizing tank again and regulate Pollutant levels in the waste water, make it kept stable (Pollutant levels are not influenced by certain special production process), to be fit to the processing condition of back operation.Detect the concentration of sulfides from wastewater.
The waste water of equalizing tank is sent into reaction tank, add ferrous sulfate (FeSO with the sulfides from wastewater equimolar amount
4) solution, under normal temperature, normal pressure, following reaction takes place:
Continue to stir, continue to produce up to no black precipitate, about 5 minutes of time, the control water PH value is 6.7;
Because the Ca in the waste water
2+Enough low, be not enough to form CaSO
4Precipitation almost is Iron sulfuret (FeS) entirely in the precipitation.
To send into settling tank through above-mentioned reacted wastewater and leave standstill, about 25 minutes of time, make the precipitation sedimentation, solid-liquid separation, (FeS) is water insoluble for Iron sulfuret, by natural subsidence, forms precipitation, is all separated; Supernatant liquor is sent acetylene generation workshop section back to and is recycled or discharge, and precipitation is sent into closed reactor;
Add dilute sulphuric acid (H to closed reactor
2SO
4), under normal temperature, normal pressure, with the precipitation in Iron sulfuret (FeS) following acidolysis reaction takes place:
Produce hydrogen sulfide (H
2S ↑) and ferrous sulfate (FeSO
4)
Press H
2SO
4: FeS=1: 1 mole number adds dilute sulphuric acid and Iron sulfuret precipitation continuously.Sulfuric acid concentration 30%, for making reaction thoroughly, reaction time 25 minutes, the pH value of controlled liq are 3;
With ferrous sulfate (FeSO
4) solution foldback ferrous sulfate storage tank, be used for acetylene sludge wastewater and handle; Hydrogen sulfide (H
2S ↑) the bulk absorption device processing of supplying gas.
Stink damp body and function liquid caustic soda (NaOH content is 33%) absorbs.The concrete practice is: countercurrent spray absorbs, and promptly sprays liquid caustic soda downwards from the absorption unit top, and gas is sent at the bottom of tower.Gas, liquid fully contact, absorbing hydrogen sulphide (H
2S ↑), following reaction takes place:
Generate sodium sulphite (Na
2S), be packaged as product after the drying.
Sodium hydroxide concentration is pressed H
2S: NaOH=1: 2 moles of meterings.
Or with hydrogen sulfide (H
2S) be oxidized to elemental sulfur, method is: with hydrogen sulfide (H
2S) send into airtight oxidation unit, aerating oxygen (O
2) oxidation, following reaction takes place:
Make elemental sulfur (S), be packaged as product after the drying.
Also can be by H
2S: NaOH=1: 1 mole is metered into sodium hydroxide, and following reaction takes place:
Generate Sodium sulfhydrate (NaHS), be packaged as product after the drying.
Embodiment two uses the zinc sulfate sedimentation
The waste water of equalizing tank is sent into reaction tank, add zinc sulfate (ZnSO with the sulfides from wastewater equimolar amount
4) solution, under normal temperature, normal pressure, following reaction takes place:
Continue to stir, continue to produce up to no white precipitate, about 5 minutes of time, the control water PH value is 6.7;
To send into settling tank through above-mentioned reacted wastewater and leave standstill, about 25 minutes of time, make the precipitation sedimentation, solid-liquid separation because zinc sulphide (ZnS) is water insoluble, is passed through natural subsidence, all separated, supernatant liquor is sent acetylene generation workshop section back to and is recycled or discharge, and precipitation is sent into closed reactor;
Add dilute sulphuric acid (H to closed reactor
2SO
4), under normal temperature, normal pressure, with the precipitation in zinc sulphide (ZnS) following acidolysis reaction takes place:
Produce hydrogen sulfide (H
2S ↑) and zinc sulfate (ZnSO
4)
Press H
2SO
4: ZnS=1: 1 mole number continues to add dilute sulphuric acid, dilute sulphuric acid concentration 40%, and for making reaction thoroughly, reaction time 25 minutes, the pH value of controlled liq are 3;
With zinc sulfate (ZnSO
4) solution foldback zinc sulfate storage tank, use for reaction tank; Hydrogen sulfide (H
2S ↑) the bulk absorption device processing of supplying gas.
Stink damp body and function liquid caustic soda (NaOH content is 33%) absorbs.The concrete practice and chemical process are with embodiment one.
Embodiment three uses the hydrochloride sedimentation
The waste water of equalizing tank is sent into reaction tank, add iron protochloride (FeCl with the sulfides from wastewater equimolar amount
2) solution, under normal temperature, normal pressure, following reaction takes place:
Continue to stir, continue to produce up to no black precipitate, about 5 minutes of time, the control water PH value is 6.9;
To send into settling tank through above-mentioned reacted wastewater and leave standstill, about 25 minutes of time, make the precipitation sedimentation, solid-liquid separation because Iron sulfuret (FeS) is water insoluble, by natural subsidence, is all separated; Supernatant liquor is sent acetylene generation workshop section back to and is recycled or discharge, and precipitation is sent into closed reactor;
Add dilute hydrochloric acid (HCl content is 25%) to closed reactor, under normal temperature, normal pressure, following acidolysis reaction take place with Iron sulfuret (FeS) in the precipitation:
Produce hydrogen sulfide (H
2S ↑) and iron protochloride (FeCl
2)
By HCl: FeS=2: 1 mole number adds hydrochloric acid continuously, and for making reaction thoroughly, reaction time 25 minutes, the pH value of controlled liq are 3;
With iron protochloride (FeCl
2) solution foldback iron protochloride storage tank, be used for acetylene sludge wastewater and handle; Hydrogen sulfide (H
2S ↑) the bulk absorption device processing of supplying gas.
Stink damp body and function liquid caustic soda (NaOH content is 33%) absorbs.The concrete practice and chemical process are with embodiment one.
Claims (7)
1. method for treating sawage generated by preparing carbide slag makes the pollutent in the acetylene sludge wastewater form precipitation with the divalent sulfur hydrochlorate or the hydrochloride of iron or zinc or copper, and liquid-solid phase is separated, and liquid phase is sent acetylene back to and workshop section takes place recycled or discharge; The solid phase precipitation thing is through acidolysis, secondary metal salt and reclaim sulphur, and concrete steps are as follows:
(1). reaction tank is gone in wastewater collection, the iron of molar equivalents such as adding and sulfides from wastewater or the divalent sulfur hydrochlorate or the hydrochloride of zinc or copper react under normal temperature, normal pressure, generate the metallic sulfide of Iron sulfuret or zinc sulphide or cupric sulfide, continue to stir, do not continue to produce up to there being precipitation;
(2). will send into the settling tank sedimentation through above-mentioned reacted wastewater, solid-liquid separation, supernatant liquor is sent acetylene generation workshop section back to and is recycled or discharge, and precipitation is sent into closed reactor;
(3). dilute sulphuric acid or hydrochloric acid to molar equivalents such as closed reactor adding and metallic sulfides under normal temperature, normal pressure, with the metallic sulfide reaction in the precipitation, generate hydrogen sulfide and ferrous salt or zinc salt or mantoquita, till no longer including the gas generation;
(4). hydrogen sulfide is sent into gas-holder; The liquid metal salts solution turns back to the metal-salt storage tank, is used for the reaction of step (1);
(5). hydrogen sulfide is prepared into sulphur or sulfide product.
2. method according to claim 1 is characterized in that, described hydrogen sulfide is prepared into sulphur or sulfide product, is preparation elemental sulfur or sodium sulphite or Sodium sulfhydrate.
3. method according to claim 2 is characterized in that, the described step that hydrogen sulfide is prepared into sodium sulphite is: hydrogen sulfide is sent into gas absorbing device, and press H
2S: NaOH=1: 2 mole numbers sodium hydroxide solution absorbing hydrogen sulphide, generate sodium sulphite, dry packing is a product.
4. method according to claim 2 is characterized in that, the described step that hydrogen sulfide is prepared into Sodium sulfhydrate is: hydrogen sulfide is sent into gas absorbing device, and press H
2S: NaOH=1: 1 mole number sodium hydroxide solution absorbing hydrogen sulphide, generate Sodium sulfhydrate, dry packing is a product.
5. method according to claim 1 is characterized in that, the described stirring time length of step (1) is 3～10 minutes, and the control condition of reaction is that the pH value of water body is 6.5～7.
6. method according to claim 1 is characterized in that, described dilute sulphuric acid of step (3) or hydrochloric acid, and the control condition of reaction is that the pH value of liquid phase is not less than 2.
7. method according to claim 6 is characterized in that, the concentration 10～70% of described dilute sulphuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510020250 CN1288101C (en) | 2005-01-24 | 2005-01-24 | Method for treating sawage generated by preparing carbide slag |
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|---|---|---|---|
| CN 200510020250 CN1288101C (en) | 2005-01-24 | 2005-01-24 | Method for treating sawage generated by preparing carbide slag |
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| CN1657447A CN1657447A (en) | 2005-08-24 |
| CN1288101C true CN1288101C (en) | 2006-12-06 |
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| CN (1) | CN1288101C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295358A (en) * | 2010-06-22 | 2011-12-28 | 天津滨海鼎昇环保科技工程有限公司 | Hierarchical coagulation treatment process for carbide slag wastewater |
| CN102249441B (en) * | 2011-04-21 | 2012-10-03 | 南京市环境保护科学研究院 | Resource comprehensive treatment process of alkaline residue from gasoline refining in oil refinery |
| CN103771418B (en) * | 2012-10-19 | 2016-04-13 | 湖北楚星化工股份有限公司 | A kind of method and device improving wastewater zero discharge in calcium carbide production |
| CN106565005A (en) * | 2016-10-27 | 2017-04-19 | 云南迪庆有色金属有限责任公司 | High-sulfur floatation wastewater treatment and sodium sulfide recycling preparation method |
| CN109354264A (en) * | 2018-12-17 | 2019-02-19 | 浙江奇彩环境科技股份有限公司 | A kind of minimizing technology of sulfur-bearing organic wastewater foul odour |
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Assignee: Sichuan Province Jinlu Resin Co., Ltd. Assignor: Yu Sunpei Contract record no.: 2010510000128 Denomination of invention: Method for treating sawage generated by preparing carbide slag Granted publication date: 20061206 License type: Exclusive License Open date: 20050824 Record date: 20101129 |
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