CN100463855C - New method of producing sodium sulfite and sodium sulfide using alkali sulfide reduction waste water - Google Patents
New method of producing sodium sulfite and sodium sulfide using alkali sulfide reduction waste water Download PDFInfo
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- CN100463855C CN100463855C CNB2006100971985A CN200610097198A CN100463855C CN 100463855 C CN100463855 C CN 100463855C CN B2006100971985 A CNB2006100971985 A CN B2006100971985A CN 200610097198 A CN200610097198 A CN 200610097198A CN 100463855 C CN100463855 C CN 100463855C
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Abstract
The present invention relates to a new method for producing sodium sulfite and sodium sulfide by using sulfur alkali reduced waste water. Said method includes the following steps: using sulfur alkali reduced waste water as mother liquor, vacuum evaporating mother liquor water, vacuum concentrating desalted or saltless mother liquor water to obtain the mixture of sodium sulfite and sodium sulfide; preparing saturated solution of said mixture; using active carbon to make adsorption and decolouring, press-filtering and removing residue; further vacuum evaporating said saturated solution whose residue is removed so as to obtain white anhydrous sodium sulfite; heating concentrating or evaporating the residual solution so as to obtain sodium sulfide.
Description
Technical field
The present invention relates to wastewater from chemical industry purifying treatment reutilization technology, particularly utilize sodium sulfide reducing waste water to produce the method for S-WAT and sodium sulphite.
Background technology
The production of many Chemicals all may produce sodium sulfide reducing waste water, for example: Chemicals such as Para-Anisidine, O-Phenylene Diamine all are to adopt the sodium sulfide reducing method to make, in process of production, must produce high density, with serious pollution sodium sulfide reducing waste water.At present, handling the modal method of sodium sulfide reducing waste water is to utilize the effective constituent adding sulphur in the waste water to carry out oxidizing reaction, produces the Sulfothiorine product then.But in this process, still have the three wastes to produce, for example: the trade effluent of sulfurous gas and hydrogen sulfide, salt slag and solid organic waste substances and COD value severe overweight etc.Therefore the purifying treatment of sodium sulfide reducing waste water is the problem that expectation is solved in the industry always.The applicant has proposed the patent application (application number 200610041069.4) of " a kind of method of purifying treatment o-phenylenediamine sodium sulfide reduction wastewater " in July, 2006, be exploration, study the just novel method of the purifying treatment sodium sulfide reducing waste water of achieving success of pilot scale practice from lab scale through in a few years.But this method is the purifying treatment o-phenylenediamine sodium sulfide reduction wastewater not only, also is applicable to the purifying treatment of the sodium sulfide reducing waste water that other Chemicals are produced in process of production.For example, can be to the purifying treatment of the sodium sulfide reducing waste water of producing Para-Anisidine, all include Sodium Sulphide, sodium hydroxide, Sulfothiorine because produce the main chemical substance composition of Para-Anisidine and the production sodium sulfide reducing waste water that O-Phenylene Diamine produced.Therefore, also basically identical of technical process, method steps that we can say their purifying treatment.Thereby this way is communicating aspect the sodium sulfide reducing waste water handling, just when in the waste water when the content of contained material and component thereof has difference, its processing step and parameter adjust possibly slightly.Described 200610041069.4 application cases have fundamentally solved the purifying treatment problem of sodium sulfide reducing waste water, non-secondary pollution produces in its treating processes, method is simple and practical, under the situation of not adding any industrial chemicals, obtain requisite raw material---the S-WAT mixture of paper industry simultaneously, also realized the production of resource utilization with sulphite manufactured paper pulp.But the S-WAT mixture new problem also occurred in being used by manufacturer, the one, and this S-WAT mixture is grey black, is unfavorable for the bleaching of paper pulp, and in treating processes, what also can produce secondary pollution; The 2nd, the component metering that this sulfurous sodium mixture provides is unstable, has increased the trouble when using; The 3rd, this S-WAT mixture also belongs to crude product, and the market general context is wideless, and the sale added value is not high.
Summary of the invention
The present invention is directed to above-mentioned existing problems, a kind of method of utilizing sodium sulfide reducing waste water to produce S-WAT and sodium sulphite has been proposed, purpose is sodium sulfide reducing waste water is done deeply to handle, purification S-WAT mixture, and obtain applied widely, be user-friendly to S-WAT that high added value, purity are higher relatively and sodium sulphite product.
Technical solution of the present invention:
The present invention is in order to make S-WAT, and the mother liquor of Sodium Sulphide is sodium sulfide reducing waste water, and the major ingredient that it comprised is Sodium Sulphide (Na
2S), sodium hydroxide (NaOH), Sulfothiorine (Na
2S
2O
3), in addition, also comprised organic matters matter.
The present invention according to the equation of chemical principle is:
3Na
2S
2O
3+ 6NaOH=2Na
2S+4Na
2SO
3+ 3H
2O detects the sodium thiosulfate content in the sodium sulfide reducing waste water, adds corresponding sodium hydroxide and reacts and obtain the S-WAT mixture, and its processing step is:
(1) vacuum-evaporation mother liquor;
(2) remove mother liquor institute sodium chloride-containing (as in the mother liquor not sodium chloride-containing can not establish this step);
(3) vacuum concentration desalination or salt-free mother liquor obtains the mixture of S-WAT and sodium sulphite;
(4) mixture of dissolving S-WAT and sodium sulphite obtains saturated solution;
(5) saturated solution decolours with charcoal absorption, and press filtration is slagged tap;
(6) saturated solution after will slagging tap carries out vacuum-evaporation, obtains the S-WAT crystallisate;
(7) above-mentioned surplus liquid is heated concentrated or evaporation, obtain the sodium sulphite crystallisate.
(1) of above processing step to the major technique feature of (three) step and 20061041069.4 application case be corresponding to.
Beneficial effect of the present invention:
(1) to " in the production of class Chemicals such as Para-Anisidine and O-Phenylene Diamine, a large amount of high density that is produced, the waste water of heavily contaminated can carry out purifying treatment completely, and non-secondary pollution produces, and has improved people's production and living environment;
(2) utilize sodium sulfide reducing waste water, under the situation of not adding any industrial chemicals, produce scope of application S-WAT wider, that purity is higher and sodium sulphite Chemicals, select usefulness for industrial enterprise, having improved the added value with regard to wastewater treatment gained byproduct, is a kind of processing method that turns waste into wealth;
(3) simple, the cleaning of whole processing step, processing sodium sulfide reducing waste water input is little, energy consumption is low, is easy to apply.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention
Embodiment
Embodiment:
The present invention produces S-WAT with the Para-Anisidine sodium sulfide reducing waste water and sodium sulphite is that example further specifies technical solution of the present invention:
In the Para-Anisidine sodium sulfide reducing waste water, main component is:
Component: sodium sulphite (Na
2S) mass concentration/(g.L
-1): 30-40
Sulfothiorine (Na
2S
2O
3) 260-280
Sodium hydroxide (NaOH) 120-130
Organism 2-3
Sodium chloride-containing not
Now in conjunction with the accompanying drawings, illustrate that again its concrete processing step is as follows:
(1) filtrated stock (being sodium sulfide reducing waste water).Remove the floating matter in the mother liquor, adopt the pressure filter press filtration, providing pressure is 110-120kPa, and press filtration goes out the organism that contains in the mother liquor.
(2) vacuum-evaporation.The mother liquor amount accounts for 60% of evaporator capacity, is no more than total volume 60%, and vacuum tightness is 80-90kPa, stops evaporation when mother liquid concentration reaches 50-55 degree Beaume, collects vapour condensation water simultaneously, makes the water coolant of cleaning in order to the back operation and uses.
(3) vacuum concentration.Earlier the vacuum-evaporation gains are emitted, detect the wherein content of Sulfothiorine and sodium hydroxide, weight 2:1 ratio requirement by contained Sulfothiorine and sodium hydroxide adds sheet or liquid sodium hydroxide, and satisfying the Sulfothiorine component is 2, and the sodium hydroxide component is 1; In the concentration tank of vacuum scraper-type, concentrate then,, when temperature reaches 135 ℃-145 ℃, eliminate vacuum, stop to concentrate when vacuum tightness reaches 80-85kPa.Emit material while hot, be deposited into the cool place, lucifuge is kept away the water part, and stack and highly be no more than 30cm, naturally cooling promptly gets the mixture of S-WAT and sodium sulphite.In spissated process, also collect vapour condensation water simultaneously, make the water coolant of cleaning in order to the back operation and use.
(4) produce S-WAT, sodium sulphite respectively.
(1) S-WAT produces.Collect in the above-mentioned operation and evaporate, the surplus water that water of condensation in the concentration process is made supercooled water again comes together in the container, the mixture of S-WAT after pulverizing and sodium sulphite is poured in this water receptacle with per 1 cubic metre of water adding 400kg ratio, stir on the limit, the limit heating, during state of saturation, put into 3-6kg ratio in per 1 cube of water again and put into gac, fully stir again, assorted by pressure filter decolouring filter then, solution after the press filtration is carried out vacuum-evaporation again, in evaporative process, along with the increase of concentration, S-WAT begins crystallization, when vacuum tightness reaches 80-90kpa, when mass concentration reaches 58-60%, eliminate vacuum, stop steam.The gained material is crystalloid S-WAT, and this material is carried out centrifugation, and with 250 ℃ of dry sodium sulphite anhydrous 99.3s that get content in the white powder more than 92% of-300 ℃ of steam flows.
(2) the producing of sodium sulphite (two kinds of methods are arranged).
(a) method places concentration tank continue to concentrate above-mentioned solution after the centrifugation of S-WAT material, and temperature reaches 140 ℃-145 ℃, and when vacuum tightness reached 80-90kpa, thick material became solid-state, pulverize content at the sodium sulphite more than 60%;
(b) method is 38-39% with above-mentioned solution evaporation after the centrifugation of S-WAT material to mass concentration, when Tc 65 is spent, kept 3-4 hours, and separated with whizzer again, promptly obtain uniform particles, stay-in-grade content at the sodium sulphite more than 60%.
In addition: need remove the step of mother liquor institute sodium chloride-containing at other the sodium sulfide reducing waste water of sodium chloride-containing, this step makes that the mother liquor temperature remains between 60-90 degree, quiescent settling 2-2.5 hours, dry through whizzer, the finished product Industrial Salt.
To sum up, the whole operation of utilizing sodium sulfide reducing waste water to produce S-WAT and sodium sulphite does not have three wastes generation.Therefore; can think: all Chemicals are produced and the sodium sulfide reducing waste water of generation with the sodium sulfide reducing method; all can the inventive method make purifying treatment, and can make S-WAT, sodium sulphite product simultaneously respectively, this also is the scope of protection of present invention.
Claims (10)
1. utilize sodium sulfide reducing waste water to produce the method for S-WAT and sodium sulphite, it is characterized in that: the sodium sulfide reducing waste water of this method utilization is the mother liquor that comprises sodium sulphite, sodium hydroxide and Sulfothiorine, and the key step of this method is: (one) vacuum-evaporation mother liquor; (2) vacuum concentration mother liquor, the mixture of acquisition S-WAT and sodium sulphite; (3) mixture of dissolving S-WAT and sodium sulphite obtains saturated solution; (4) saturated solution decolours with charcoal absorption, and press filtration is slagged tap; (5) saturated solution after will slagging tap carries out vacuum-evaporation, obtains the S-WAT crystallisate; (6) above-mentioned surplus liquid is heated concentrated or evaporation acquisition sodium sulphite crystallisate.
2. the sodium sulfide reducing waste water that utilizes according to claim 1 is produced S-WAT and sodium sulphite method, it is characterized in that: when containing the sodium-chlor component in the mother liquor, need to remove the step of institute's sodium chloride-containing in the mother liquor between above-mentioned steps () and the step (two).
3. the sodium sulfide reducing waste water that utilizes according to claim 1 is produced S-WAT and sodium sulphite method, it is characterized in that: also comprise the mother liquor filtration step before the described vacuum-evaporation mother liquor; Also comprise the treatment step that concentrates material after the described vacuum concentration mother liquor, promptly emit material while hot, be deposited into the cool place, lucifuge is kept away the water part, and stack and highly be no more than 30cm, naturally cooling promptly gets the mixture of S-WAT and sodium sulphite.
4. the method for utilizing sodium sulfide reducing waste water to produce S-WAT and sodium sulphite according to claim 1, it is characterized in that: in the described vacuum-evaporation mother liquor step, the mother liquor amount accounts for 60% of evaporator capacity, vacuum tightness is 80-90kPa, when reaching 50-55 degree Beaume, mother liquid concentration stops evaporation, collect vapour condensation water simultaneously, as the water coolant of back operation.
5. the method for utilizing sodium sulfide reducing waste water to produce S-WAT and sodium sulphite according to claim 2, it is characterized in that: the described step that removes mother liquor institute sodium chloride-containing, need make the mother liquor temperature remain on quiescent settling 2-2.5 hours between 60-90 degree, dry through whizzer, get the finished product Industrial Salt.
6. the method for utilizing sodium sulfide reducing waste water to produce S-WAT and sodium sulphite according to claim 1, it is characterized in that: described vacuum concentration mother liquor step is earlier the vacuum-evaporation gains to be emitted, detect the wherein content of Sulfothiorine and sodium hydroxide, weight 2:1 ratio requirement by contained Sulfothiorine and sodium hydroxide, add sodium hydroxide, in the concentration tank of vacuum scraper-type, concentrate then, when vacuum tightness reaches 80-85kPa, when temperature reaches 135 ℃-145 ℃, eliminate vacuum, stop to concentrate.
7. the sodium sulfide reducing waste water that utilizes according to claim 1 is produced S-WAT and sodium sulphite method, it is characterized in that: the mixture of described dissolving S-WAT and sodium sulphite, obtain saturated solution, decolour with charcoal absorption, press filtration is slagged tap, and the solution after the press filtration is carried out vacuum-evaporation again, obtains the crystallization S-WAT, whizzer separates again, gets sodium sulphite anhydrous 99.3; To get sodium sulphite through solution reconcentration or the revaporization after the centrifugation of S-WAT material.
8. the method for utilizing sodium sulfide reducing waste water to produce S-WAT and Sodium Sulphide according to claim 7, it is characterized in that: the concrete steps that obtain S-WAT are the mixtures with S-WAT and Sodium Sulphide, stir with limit in the water of 1 cubic metre of every 400kg adding, the limit heating, put into 3-6kg ratio in per 1 cube of water again and put into gac, fully stir again, assorted by pressure filter decolouring filter then, solution after the press filtration is carried out vacuum-evaporation again, in evaporative process, along with the increase of concentration, S-WAT begins crystallization, when vacuum tightness reaches 80-90kPa, when mass concentration reaches 58-60%, eliminate vacuum, stop steam,, carry out centrifugation crystalloid S-WAT, and, get sodium sulphite anhydrous 99.3 with 250 ℃ of-300 ℃ of steam flow dryings.
9. the method for utilizing sodium sulfide reducing waste water to produce S-WAT and sodium sulphite according to claim 7, it is characterized in that: will be through the solution after the centrifugation of S-WAT material, the concrete steps that obtain sodium sulphite with concentration method are to make thickening temperature reach 140 ℃-145 ℃, vacuum tightness reaches 80-90kPa, thick material promptly becomes solid-state, pulverize Sodium Sulphide; The concrete steps that obtain Sodium Sulphide with method of evaporating are that to make solution evaporation be 38-39% to mass concentration, when Tc 65 is spent, keep 3-4 hours, separate with whizzer again, must sodium sulphite.
10. the method for utilizing sodium sulfide reducing waste water to produce S-WAT and Sodium Sulphide according to claim 1, it is characterized in that: described sodium sulfide reducing waste water is the sodium sulfide reducing waste water of Para-Anisidine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100971985A CN100463855C (en) | 2006-10-31 | 2006-10-31 | New method of producing sodium sulfite and sodium sulfide using alkali sulfide reduction waste water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100971985A CN100463855C (en) | 2006-10-31 | 2006-10-31 | New method of producing sodium sulfite and sodium sulfide using alkali sulfide reduction waste water |
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| Publication Number | Publication Date |
|---|---|
| CN1948153A CN1948153A (en) | 2007-04-18 |
| CN100463855C true CN100463855C (en) | 2009-02-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100971985A Expired - Fee Related CN100463855C (en) | 2006-10-31 | 2006-10-31 | New method of producing sodium sulfite and sodium sulfide using alkali sulfide reduction waste water |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115114B (en) * | 2010-12-31 | 2013-01-02 | 谢善情 | Method for preparing copper sulfide, calcium carbonate and sodium hydroxide from sodium sulfide waste |
| CN104086440A (en) * | 2014-06-10 | 2014-10-08 | 安徽华润涂料有限公司 | Technology for processing mother liquor of o-phenylenediamine |
| CN104310432B (en) * | 2014-09-30 | 2015-10-28 | 哈尔滨工业大学 | A kind of method of sodium-chlor and five water Sulfothiorine in Crystallization Separation waste residue |
| CN108249462B (en) * | 2018-02-06 | 2020-03-24 | 中国中轻国际工程有限公司 | Process for producing sodium sulfide and sodium sulfate from sodium sulfide dilute solution and sodium sulfate decahydrate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB915734A (en) * | 1960-08-03 | 1963-01-16 | Stora Kopparbergs Bergslags Ab | Improved method for the recovery of chemicals out of waste lyes from the manufactureof cellulose |
| GB1328920A (en) * | 1968-10-30 | 1973-09-05 | Ebara Infilco | Method for converting sodium sulphide to sodium sulphite |
-
2006
- 2006-10-31 CN CNB2006100971985A patent/CN100463855C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB915734A (en) * | 1960-08-03 | 1963-01-16 | Stora Kopparbergs Bergslags Ab | Improved method for the recovery of chemicals out of waste lyes from the manufactureof cellulose |
| GB1328920A (en) * | 1968-10-30 | 1973-09-05 | Ebara Infilco | Method for converting sodium sulphide to sodium sulphite |
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