CN101913625A - Method for preparing caustic soda, calcium carbonate, sodium thiosulfide and sodium iodide from sodium sulphide waste slag - Google Patents
Method for preparing caustic soda, calcium carbonate, sodium thiosulfide and sodium iodide from sodium sulphide waste slag Download PDFInfo
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- CN101913625A CN101913625A CN 201010243985 CN201010243985A CN101913625A CN 101913625 A CN101913625 A CN 101913625A CN 201010243985 CN201010243985 CN 201010243985 CN 201010243985 A CN201010243985 A CN 201010243985A CN 101913625 A CN101913625 A CN 101913625A
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Abstract
The invention discloses a method for preparing caustic soda, calcium carbonate, sodium thiosulfide and sodium iodide from sodium sulfide waste slag, which comprises: reacting calcium hydroxide with sodium and sodium carbonate in the sodium sulfide waste slag to obtain mixture of sodium hydroxide, calcium carbonate and calcium sulfide, filtering to separate the sodium hydroxide from the mixture, adding sodium carbonate into the mixture of the calcium carbonate and the calcium sulfide to convert the calcium sulfide into calcium carbonate and sodium sulfide, filtering to separate the calcium carbonate from the sodium sulfide, mixing and reacting the sodium sulfide with sodium sulfate and iodine to obtain mixed solution of sodium thiosulfate and sodium iodide, distilling the mixed solution under reduced pressure to obtain saturated solution, cooling with temperature control to precipitate sodium iodide first, filtering under vacuum, separating to obtain a sodium iodide product, and drying filtrate which contains saturated solution of sodium thiosulfate by spraying to obtain a sodium thiosulfate product. The method eliminates the pollution caused by the sodium sulfide in the alkali sulfide waste slag to the environment, effectively utilizes the potential values of the alkali sulfide waste slag, changes waste into valuable materials and is a method of high practical value.
Description
Technical field
The present invention relates to the improvement of barium sulfate by-product sodium sulfide method gained Sodium Sulphide waste residue and the technical field of utilization, particularly, relate to the method for preparing caustic soda, lime carbonate, Sulfothiorine and sodium iodide with the Sodium Sulphide waste residue.
Background technology
The industrial process of Sodium Sulphide (sodium sulphite) mainly contains coal dust reduction of mirabilite method, gas reduction method, barium sulfate by-product sodium sulfide method and hydrogen sulfide method.Wherein, barium sulfate by-product sodium sulfide method is to produce barium sulphide with coal reduction barium sulfate, adds metabisulfite solution again and handles, and generates sodium sulphite and process white, separates evaporation concentration and getting through suction filtration.This method is discharged a large amount of Sodium Sulphide waste residues, and is wherein most of from carbon contained in the coal, and fails isolating sodium sulphite.After testing, the content of yellow soda ash in this Sodium Sulphide waste residue reaches 12-15%, and sodium sulphite is 25-30%.
Total institute is known, and sodium sulphite is very easily water-soluble, and the aqueous solution is strong basicity, and extremely strong pungency and corrodibility are arranged when contacting with mucous membrane with skin, can cause when touching skin and hair and burn.Especially react the hydrogen sulfide that generates with water, behind the absorption human body, thereby cause the extremely death of poisoning, therefore,, not only can cause environmental pollution, also have certain potential safety hazard if the Sodium Sulphide waste residue is not used and administers.
Yet, about the comprehensive utilization and the improvement of Sodium Sulphide waste residue, at present, not having feasible method, producer's majority of production Sodium Sulphide waste residue is directly stacked the Sodium Sulphide waste residue or is buried, and this is undoubted, can cause very serious environmental pollution and deterioration.
Therefore, be necessary to explore the method for from the Sodium Sulphide waste residue, extracting sodium sulphite, thereby effectively excavate the potential value of Sodium Sulphide waste residue, eliminate environmental pollution and potential safety hazard.For this reason, the applicant has explored the method for preparing caustic soda, lime carbonate, sodium sulphite and sodium iodide with the Sodium Sulphide waste residue, and this method effectively is converted into utilizable material with the effective constituent in the Sodium Sulphide, has very great economic implications.
Wherein, caustic soda is soluble in water, is strong basicity, and the Na+ ion can both be provided.These character are widely used in all departments such as soap system, weaving, printing and dyeing, bleaching, papermaking, turpentole, metallurgy and other chemical industry them, are a kind of important chemical material.
Lime carbonate is a kind of important raw mineral materials, can be used as the filler of industries such as rubber, plastics, papermaking, coating and printing ink.Be widely used in the productions such as organic synthesis, metallurgy, glass and asbestos.Also can be used as middle kind of agent, the gastroduodenal ulcer disease of trade effluent antacid, acidosic toxinicide, contain the release agent of SO2 remover, dairy feed compound and tar felt in the SO2 waste gas.The raw material that also can be used as tooth powder, toothpaste and other makeup.
The purposes of Sulfothiorine is very extensive, is mainly used in photography and makes fixing salt.Dechlorinating agent when the SYNTHETIC OPTICAL WHITNER of the neutralizing agent of the reductive agent of dichromate, nitrogenous tail gas when next does tanning, mordant, straw and hair and association with pulp bleaching.Also be used for the manufacturing of tetraethyllead, dyestuff intermediate etc. and ore desilver etc.
And sodium iodide in pharmaceutical industry, as the raw material of analytical reagent and preparation monocrystalline, also is used as the raw material of all kinds of iodine compounds of preparation as the solubility promoter of analytical reagent and iodine.
Summary of the invention
The objective of the invention is to, the method for preparing caustic soda, lime carbonate, Sulfothiorine and sodium iodide with the Sodium Sulphide waste residue is provided, this method turns waste into wealth, and has eliminated the pollution of Sodium Sulphide waste residue to environment.
Technical scheme of the present invention is as follows: prepare caustic soda with the Sodium Sulphide waste residue, lime carbonate, the method of Sulfothiorine and sodium iodide, with sodium sulphite in calcium hydroxide and the Sodium Sulphide waste residue and yellow soda ash reaction, make sodium hydroxide, lime carbonate and sulfurated lime mixture, after filtration sodium hydroxide is separated from mixture, then in lime carbonate and sulfurated lime mixture, add yellow soda ash again, thereby sulfurated lime is converted into lime carbonate and sodium sulphite, after filtration lime carbonate is separated with sodium sulphite again, with sodium sulphite and sodium sulfate and iodine hybrid reaction, obtain Sulfothiorine and sodium iodide mixed solution, the gained mixed solution arrives saturated solution through underpressure distillation, temperature control cooling again, sodium iodide is separated out earlier, behind the suction filtration, separate to obtain the sodium iodide product, and it is spray-dried to contain the filtrate of Sulfothiorine saturated solution, obtain the Sulfothiorine product, comprise following concrete steps:
Steps A: the content of sodium sulphite and yellow soda ash in the conversion Sodium Sulphide waste residue, and configuration Sodium Sulphide waste residue suspension liquid and aqua calcis;
Step B: is 1: 0.5～1 successively to drop into first protection against corrosion reactor (1) lining with Sodium Sulphide waste residue suspension liquid and aqua calcis with the ratio of the molar weight sum of the pure substance of sodium sulphite and yellow soda ash and the molar weight of calcium hydroxide, carry out chemical reaction, obtain containing the mixture of sodium hydroxide, lime carbonate and sulfurated lime;
Step C: step B gained mixture is filtered through first strainer (2), filter the clarifying filter cake that contains the solution of hydrogen-oxygen sodium and contain lime carbonate and sulfurated lime mixture;
Step D: the solution that contains hydrogen-oxygen sodium that step C is obtained sends into that air distillation is blocky sodium hydroxide product (4) in first distiller (3);
Step e: the filter cake that contains lime carbonate and sulfurated lime mixture that step C is obtained washs through first washing machine (5), obtain carbon/sulfur calcium mixture crude product (6), through first drying machine (7) drying, first pulverizer (8) is pulverized, and obtains carbon/sulfur calcium mixture finished product (9) with carbon/sulfur calcium mixture crude product (6);
Step F: configuration sodium carbonate solution, step e gained carbon/sulfur calcium mixture finished product (9) and sodium carbonate solution are successively dropped in the second protection against corrosion reactor (10) with sulfurated lime and the pure mass ratio of yellow soda ash 1: 1.27～1.67, slowly stir and carry out chemical reaction, generate the mixture that contains lime carbonate and sodium sulphite;
Step G: the mixture that contains lime carbonate and sodium sulphite of step F gained is filtered through second strainer (11), filter the solution and the filter cake calciferous of clarifying Containing Sulfur sodium;
Step H: filter cake calciferous is washed through second washing machine (12), second drying machine (13) drying, second pulverizer (14) is pulverized, and obtains lime carbonate finished product (15);
Step I: dispose metabisulfite solution and iodine solution respectively, is 1: 1～1.3: 1.6～2.1 to send into reaction in the 3rd protection against corrosion reactor (16) with the solution of the Containing Sulfur sodium of step G gained and metabisulfite solution and iodine solution according to the ratio of sodium sulphite and the pure substance quality of sodium sulfate and iodine, obtains containing the mixture of Sulfothiorine and sodium iodide;
Step J: the mixture that contains Sulfothiorine and sodium iodide of step I gained is dropped into distillation in the underpressure distillation device (17), make through temperature control cooler (18) and cool off, the crystallization of sodium iodide elder generation is separated out, and after behind the 3rd suction filtration machine (19) suction filtration, obtain containing the crystal and the solution that contains Sulfothiorine of sodium iodide;
Step K: the crystal that contains sodium iodide of step J gained is dried, pulverizes, packs, obtain sodium iodide product (20);
Step L: the solution that contains Sulfothiorine of step J gained is sent into the middle solution that reaches capacity that distills of the 3rd distiller (21), use the 3rd spray-dryer (22) drying again, obtain powder Sulfothiorine product (23).
Described Sodium Sulphide waste residue is the product with barium sulfate by-product sodium sulfide method gained.
Before the configuration Sodium Sulphide waste residue suspension liquid, earlier described Sodium Sulphide waste residue is ground into 40 orders.
The described chemical reaction of step B carries out under slowly stirring.
Washings retrieval system recycling after the step e washing.
Washings retrieval system recycling after the step I washing.
The principle of chemical reaction involved in the present invention is:
Na
2S+Ca(OH)
2＝＝＝＝＝2NaOH+CaS
Na
2CO
3+Ca(OH)
2＝＝＝＝＝2NaOH+CaCO
3
CaS+Na
2CO
3＝＝＝＝＝CaCO
3+Na
2S
5Na
2S+3Na
2SO
4+4I
2＝＝＝＝＝4Na
2S2
O3
+8NaI
The invention has the beneficial effects as follows: the method for preparing caustic soda, lime carbonate, Sulfothiorine and sodium iodide with the Sodium Sulphide waste residue of the present invention, this method will be converted into industrial raw material caustic soda, lime carbonate, Sulfothiorine and sodium iodide with the Sodium Sulphide waste residue of barium sulfate by-product sodium sulfide method gained, thereby eliminated in the Sodium Sulphide waste residue sodium sulphite to the pollution of environment, effectively utilized the potential value of Sodium Sulphide waste residue, having realized turning waste into wealth, is a method of great practical value.
Description of drawings
Fig. 1 prepares the process flow sheet of the method for caustic soda, lime carbonate, Sulfothiorine and sodium iodide for of the present invention with the Sodium Sulphide waste residue, wherein,
(1)---the first protection against corrosion reactor, (2)---first strainer, (3)---first distiller, (4)---sodium hydroxide product, (5)---first washing machine, (6)---the carbon/sulfur calcium mixture crude product, (7)---first drying machine, (8)---first pulverizer, (9)---carbon/sulfur calcium mixture product, (10)---the second protection against corrosion reactor, (11)---second strainer, (12)---second washing machine, (13)---second drying machine, (14)---second pulverizer, (15) lime carbonate finished product, (16)---the 3rd protection against corrosion reactor, (17)---underpressure distillation device, (18)---the temperature control cooler, (19)---the 3rd suction filtration machine, (20)---sodium iodide product, (21)---the 3rd distiller, (22)---the 3rd spray-dryer, (23)---powder Sulfothiorine product.
Embodiment
With reference to Fig. 1, the method for preparing caustic soda, lime carbonate, Sulfothiorine and sodium iodide with the Sodium Sulphide waste residue, take by weighing the Sodium Sulphide waste residue of certain station-service barium sulfate by-product sodium sulfide method gained, convert that sodium sulphite quality percentage composition is 25% in this Sodium Sulphide waste residue, yellow soda ash quality percentage composition is 15%, take by weighing Sodium Sulphide waste residue 500kg, and calculate the molar weight of sodium sulphite and yellow soda ash in the Sodium Sulphide waste residue waste residue of described weighing, it is 40 purpose powder that the Sodium Sulphide waste residue is pulverized, then, Sodium Sulphide waste residue and water is miscible, be configured to Sodium Sulphide waste residue suspension liquid; Simultaneously the ratio according to the molar weight sum of sodium sulphite and yellow soda ash and the molar weight of calcium hydroxide is 1: 1 configuration aqua calcis; Sodium Sulphide waste residue suspension liquid and aqua calcis are successively dropped into protection against corrosion reactor (1) lining, carry out chemical reaction under slowly stirring, obtain containing the mixture of sodium hydroxide, lime carbonate and sulfurated lime; The gained mixture is filtered through filter (2), and filter obtains clarifying sodium hydroxide solution, contains the filter cake of lime carbonate and sulfurated lime; Sodium hydroxide solution is sent into air distillation blocky sodium hydroxide product (4) in the distiller (3), and it contains the sodium hydroxide pure substance is 184.27kg; The filter cake that will contain lime carbonate and sulfurated lime is through washing machine (5) washing, obtain carbon/sulfur calcium mixture crude product (6), with carbon/sulfur calcium mixture crude product (6) drying machine (7) drying, pulverizer (8) is pulverized, obtain carbon/sulfur calcium mixture finished product (7), it contains the lime carbonate pure substance is 70.75kg, and the sulfurated lime pure substance is 115.4kg.
The configuration sodium carbonate solution, gained carbon/sulfur calcium mixture finished product (9) and yellow soda ash sodium solution are successively dropped in second protection against corrosion reactor (10) with sulfurated lime and the pure mass ratio of yellow soda ash at 1: 1.67, slowly stir and carry out chemical reaction, generate the mixture that contains lime carbonate and sodium sulphite; The mixture that contains lime carbonate and sodium sulphite of gained is filtered through second strainer (11), filter the solution and the filter cake calciferous of clarifying Containing Sulfur sodium; Containing the sodium sulphite pure substance in the solution of Containing Sulfur sodium is 125.02kg (14); Filter cake calciferous is washed through second washing machine (12), second drying machine (13) drying, second pulverizer (14) is pulverized, and obtains lime carbonate finished product (15), and the lime carbonate pure substance that it contains is 231.03kg.
Dispose metabisulfite solution and iodine solution respectively, is reaction in 1: 1: 1.6 the 3rd protection against corrosion reactor (16) with the solution of the Containing Sulfur sodium of gained and metabisulfite solution and iodine solution according to the ratio of sodium sulphite and the pure substance quality of sodium sulfate and iodine, obtains containing the mixture of Sulfothiorine and sodium iodide; With distillation in this mixture input underpressure distillation device (17), make through temperature control cooler (18) cooling, the crystallization of sodium iodide elder generation is separated out, and after behind the 3rd suction filtration machine (19) suction filtration, obtain containing the crystal and the solution that contains Sulfothiorine of sodium iodide; The crystal that will contain sodium iodide dries, pulverizes, packs, and obtains sodium iodide product 250.04kg (20); The solution that contains Sulfothiorine of gained is sent into the middle solution that reaches capacity that distills of the 3rd distiller (21), use the 3rd spray-dryer (22) drying again, obtain powder Sulfothiorine product 42.94kg (23).
Embodiment 2
With reference to Fig. 1, the method for preparing caustic soda, lime carbonate, Sulfothiorine and sodium iodide with the Sodium Sulphide waste residue, take by weighing the Sodium Sulphide waste residue of certain station-service barium sulfate by-product sodium sulfide method gained, convert that sodium sulphite quality percentage composition is 25% in this Sodium Sulphide waste residue, yellow soda ash quality percentage composition is 15%, take by weighing Sodium Sulphide waste residue 500kg, and calculate the molar weight of sodium sulphite and yellow soda ash in the Sodium Sulphide waste residue waste residue of described weighing, it is 40 purpose powder that the Sodium Sulphide waste residue is pulverized, then, Sodium Sulphide waste residue and water is miscible, be configured to Sodium Sulphide waste residue suspension liquid; Simultaneously the ratio according to the molar weight sum of sodium sulphite and yellow soda ash and the molar weight of calcium hydroxide is 1: 0.5 configuration aqua calcis; Sodium Sulphide waste residue suspension liquid and aqua calcis are successively dropped into protection against corrosion reactor (1) lining, carry out chemical reaction under slowly stirring, obtain containing the mixture of sodium hydroxide, lime carbonate and sulfurated lime; The gained mixture is filtered through filter (2), and filter obtains clarifying sodium hydroxide solution, contains the filter cake of lime carbonate and sulfurated lime; Sodium hydroxide solution is sent into air distillation blocky sodium hydroxide product (4) in the distiller (3), and it contains the sodium hydroxide pure substance is 92.14kg; The filter cake that will contain lime carbonate and sulfurated lime is through washing machine (5) washing, obtain carbon/sulfur calcium mixture crude product (6), with carbon/sulfur calcium mixture crude product (6) drying machine (7) drying, pulverizer (8) is pulverized, obtain carbon/sulfur calcium mixture finished product (7), it contains the lime carbonate pure substance is 35.28kg, and the sulfurated lime pure substance is 57.7kg.
The configuration sodium carbonate solution, gained carbon/sulfur calcium mixture finished product (9) and yellow soda ash sodium solution are successively dropped in second protection against corrosion reactor (10) with sulfurated lime and the pure mass ratio of yellow soda ash at 1: 1.47, slowly stir and carry out chemical reaction, generate the mixture that contains lime carbonate and sodium sulphite; The mixture that contains lime carbonate and sodium sulphite of gained is filtered through second strainer (11), filter the solution and the filter cake calciferous of clarifying Containing Sulfur sodium; The Containing Sulfur sodium solution is sent into the middle solution that reaches capacity that distills of after-fractionating device (12), use second spray-dryer (13) drying again, obtain powder sodium sulphite product, it contains the sodium sulphite pure substance is 62.51kg (14); Filter cake calciferous is washed through second washing machine (15), second drying machine (16) drying, second pulverizer (17) is pulverized, and obtains the lime carbonate finished product, and the lime carbonate pure substance that it contains is 115.52kg (18).
Dispose metabisulfite solution and iodine solution respectively, is reaction in 1: 1.2: 1.8 the 3rd protection against corrosion reactor (16) with the solution of the Containing Sulfur sodium of gained and metabisulfite solution and iodine solution according to the ratio of sodium sulphite and the pure substance quality of sodium sulfate and iodine, obtains containing the mixture of Sulfothiorine and sodium iodide; With distillation in this mixture input underpressure distillation device (17), make through temperature control cooler (18) cooling, the crystallization of sodium iodide elder generation is separated out, and after behind the 3rd suction filtration machine (19) suction filtration, obtain containing the crystal and the solution that contains Sulfothiorine of sodium iodide; The crystal that will contain sodium iodide dries, pulverizes, packs, and obtains sodium iodide product 140.65kg (20); The solution that contains Sulfothiorine of gained is sent into the middle solution that reaches capacity that distills of the 3rd distiller (21), use the 3rd spray-dryer (22) drying again, obtain powder Sulfothiorine product 24.16kg (23).
Embodiment 3
With reference to Fig. 1, the method for preparing caustic soda, lime carbonate, Sulfothiorine and sodium iodide with the Sodium Sulphide waste residue, take by weighing the Sodium Sulphide waste residue of certain station-service barium sulfate by-product sodium sulfide method gained, convert that sodium sulphite quality percentage composition is 25% in this Sodium Sulphide waste residue, yellow soda ash quality percentage composition is 15%, take by weighing Sodium Sulphide waste residue 500kg, and calculate the molar weight of sodium sulphite and yellow soda ash in the Sodium Sulphide waste residue waste residue of described weighing, it is 40 purpose powder that the Sodium Sulphide waste residue is pulverized, then, Sodium Sulphide waste residue and water is miscible, be configured to Sodium Sulphide waste residue suspension liquid; Simultaneously the ratio according to the molar weight sum of sodium sulphite and yellow soda ash and the molar weight of calcium hydroxide is 1: 0.7 configuration aqua calcis; Sodium Sulphide waste residue suspension liquid and aqua calcis are successively dropped into protection against corrosion reactor (1) lining, carry out chemical reaction under slowly stirring, obtain containing the mixture of sodium hydroxide, lime carbonate and sulfurated lime; The gained mixture is filtered through filter (2), and filter obtains clarifying sodium hydroxide solution, contains the filter cake of lime carbonate and sulfurated lime; Sodium hydroxide solution is sent into air distillation blocky sodium hydroxide product (4) in the distiller (3), and it contains the sodium hydroxide pure substance is 128.99kg; The filter cake that will contain lime carbonate and sulfurated lime is through washing machine (5) washing, obtain carbon/sulfur calcium mixture crude product (6), with carbon/sulfur calcium mixture crude product (6) drying machine (7) drying, pulverizer (8) is pulverized, obtain carbon/sulfur calcium mixture finished product (7), it contains the lime carbonate pure substance is 49.5kg, and the sulfurated lime pure substance is 80.7kg.
The configuration sodium carbonate solution, gained carbon/sulfur calcium mixture finished product (9) and yellow soda ash sodium solution are successively dropped in second protection against corrosion reactor (10) with sulfurated lime and the pure mass ratio of yellow soda ash at 1: 1.27, slowly stir and carry out chemical reaction, generate the mixture that contains lime carbonate and sodium sulphite; The mixture that contains lime carbonate and sodium sulphite of gained is filtered through second strainer (11), filter the solution and the filter cake calciferous of clarifying Containing Sulfur sodium; The Containing Sulfur sodium solution is sent into the middle solution that reaches capacity that distills of after-fractionating device (12), use second spray-dryer (13) drying again, obtain powder sodium sulphite product, it contains the sodium sulphite pure substance is 75.42kg (14); Filter cake calciferous is washed through second washing machine (15), second drying machine (16) drying, second pulverizer (17) is pulverized, and obtains the lime carbonate finished product, and the lime carbonate pure substance that it contains is 146.19kg (18)
Dispose metabisulfite solution and iodine solution respectively, is reaction in 1: 1.3: 2.1 the 3rd protection against corrosion reactor (16) with the solution of the Containing Sulfur sodium of gained and metabisulfite solution and iodine solution according to the ratio of sodium sulphite and the pure substance quality of sodium sulfate and iodine, obtains containing the mixture of Sulfothiorine and sodium iodide; With distillation in this mixture input underpressure distillation device (17), make through temperature control cooler (18) cooling, the crystallization of sodium iodide elder generation is separated out, and after behind the 3rd suction filtration machine (19) suction filtration, obtain containing the crystal and the solution that contains Sulfothiorine of sodium iodide; The crystal that will contain sodium iodide dries, pulverizes, packs, and obtains sodium iodide product 177.91kg (20); The solution that contains Sulfothiorine of gained is sent into the middle solution that reaches capacity that distills of the 3rd distiller (21), use the 3rd spray-dryer (22) drying again, obtain powder Sulfothiorine product 30.55kg (23).
Above content be in conjunction with concrete preferred implementation to further describing that the present invention did, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, its framework form can be flexible and changeable, can the subseries method.Just make some simple deduction or replace, all should be considered as belonging to the scope of patent protection that the present invention is determined by claims of being submitted to.
Claims (6)
1. prepare caustic soda with the Sodium Sulphide waste residue, lime carbonate, the method of sodium sulfate and sodium iodide, it is characterized in that, with sodium sulphite in calcium hydroxide and the Sodium Sulphide waste residue and yellow soda ash reaction, make sodium hydroxide, lime carbonate and sulfurated lime mixture, after filtration sodium hydroxide is separated from mixture, then in lime carbonate and sulfurated lime mixture, add yellow soda ash again, thereby sulfurated lime is converted into lime carbonate and sodium sulphite, after filtration lime carbonate is separated with sodium sulphite again,, obtain Sulfothiorine and sodium iodide mixed solution sodium sulphite and sodium sulfate and iodine hybrid reaction, the gained mixed solution arrives saturated solution through underpressure distillation, temperature control cooling again separates out sodium iodide earlier, behind the suction filtration, separate and obtain the sodium iodide product, and the filtrate that contains the Sulfothiorine saturated solution is spray-dried, obtains the Sulfothiorine product, comprises following concrete steps:
Steps A: sodium sulfide content in the conversion Sodium Sulphide waste residue, and configuration Sodium Sulphide waste residue suspension liquid and aqua calcis;
Step B: is 1: 0.5～1 successively to drop into first protection against corrosion reactor (1) lining with Sodium Sulphide waste residue suspension liquid and aqua calcis with the ratio of the molar weight sum of sodium sulphite and yellow soda ash pure substance and the molar weight of calcium hydroxide, carry out chemical reaction, obtain containing the mixture of sodium hydroxide, lime carbonate and sulfurated lime;
Step C: step B gained mixture is filtered through first strainer (2), filter the clarifying filter cake that contains the solution of hydrogen-oxygen sodium and contain lime carbonate and sulfurated lime mixture;
Step D: the solution that contains hydrogen-oxygen sodium that step C is obtained sends into that air distillation is blocky sodium hydroxide product (4) in first distiller (3);
Step e: the filter cake that contains lime carbonate and sulfurated lime mixture that step C is obtained washs through first washing machine (5), obtain carbon/sulfur calcium mixture crude product (6), through first drying machine (7) drying, first pulverizer (8) is pulverized, and obtains carbon/sulfur calcium mixture finished product (9) with carbon/sulfur calcium mixture crude product (6);
Step F: configuration sodium carbonate solution, step e gained carbon/sulfur calcium mixture finished product (9) and sodium carbonate solution are successively dropped in the second protection against corrosion reactor (10) with sulfurated lime and the pure mass ratio of yellow soda ash 1: 1.27～1.67, slowly stir and carry out chemical reaction, generate the mixture that contains lime carbonate and sodium sulphite;
Step G: the mixture that contains lime carbonate and sodium sulphite of step F gained is filtered through second strainer (11), filter the solution and the filter cake calciferous of clarifying Containing Sulfur sodium;
Step H: filter cake calciferous is washed through second washing machine (12), second drying machine (13) drying, second pulverizer (14) is pulverized, and obtains lime carbonate finished product (15);
Step I: dispose metabisulfite solution and iodine solution respectively, is 1: 1～1.3: 1.6～2.1 to send into reaction in the 3rd protection against corrosion reactor (16) with the solution of the Containing Sulfur sodium of step G gained and metabisulfite solution and iodine solution according to the ratio of sodium sulphite and the pure substance quality of sodium sulfate and iodine, obtains containing the mixture of Sulfothiorine and sodium iodide;
Step J: the mixture that contains Sulfothiorine and sodium iodide of step I gained is dropped into distillation in the underpressure distillation device (17), make through temperature control cooler (18) and cool off, the crystallization of sodium iodide elder generation is separated out, and after behind the 3rd suction filtration machine (19) suction filtration, obtain containing the crystal of sodium iodide and the solution of contains sodium sulfate;
Step K: the crystal that contains sodium iodide of step J gained is dried, pulverizes, packs, obtain sodium iodide product (20);
Step L: the solution of the contains sodium sulfate of step J gained is sent in the 3rd distiller (21) the distillation solution that reaches capacity, use the 3rd spray-dryer (22) drying again, obtain powder sodium sulfate product (23).
2. as claimed in claim 1ly prepare the method for caustic soda, lime carbonate, sodium sulfate and sodium iodide, it is characterized in that described Sodium Sulphide waste residue is the product with barium sulfate by-product sodium sulfide method gained with the Sodium Sulphide waste residue.
3. as claimed in claim 1ly prepare the method for caustic soda, lime carbonate, sodium sulfate and sodium iodide, it is characterized in that, before the configuration Sodium Sulphide waste residue suspension liquid, earlier described Sodium Sulphide waste residue is ground into 40 orders with the Sodium Sulphide waste residue.
4. as claimed in claim 1ly prepare the method for caustic soda, lime carbonate, sodium sulfate and sodium iodide, it is characterized in that the described chemical reaction of step B is carrying out under slowly stirring with the Sodium Sulphide waste residue.
5. as claimed in claim 1ly prepare the method for caustic soda, lime carbonate, sodium sulfate and sodium iodide, it is characterized in that the washings retrieval system recycling after the step e washing with the Sodium Sulphide waste residue.
6. as claimed in claim 1ly prepare the method for caustic soda, lime carbonate, sodium sulfate and sodium iodide, it is characterized in that the washings retrieval system recycling after the step I washing with the Sodium Sulphide waste residue.
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| CN101200336A (en) * | 2007-12-18 | 2008-06-18 | 赵志军 | Process for zero-discharge treatment of o-phenylenediamine sodium sulfide reduction wastewater |
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2010
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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