CN102328911A - Method for preparing sodium sulfide and barium chloride with cogeneration of powdery barium salt by using salting-out master liquid generated in zinc powder method - Google Patents
Method for preparing sodium sulfide and barium chloride with cogeneration of powdery barium salt by using salting-out master liquid generated in zinc powder method Download PDFInfo
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- CN102328911A CN102328911A CN201110142069A CN201110142069A CN102328911A CN 102328911 A CN102328911 A CN 102328911A CN 201110142069 A CN201110142069 A CN 201110142069A CN 201110142069 A CN201110142069 A CN 201110142069A CN 102328911 A CN102328911 A CN 102328911A
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Abstract
The invention belongs to the technical field of treatment and utilization of three wastes (waste gas, waste water and waste residues) in the chemical industry, and particularly relates to a method for preparing sodium sulfide and barium chloride with cogeneration of a powdery barium salt by using salting-out master liquid generated in a zinc powder method. In the invention, by mainly utilizing the salting-out master liquid, which is generated in a process of preparing sodium hydrosulfite by using the zinc powder method, for treating barium sulfide, not only can sodium sulfide, barium chloride and powdery barium salt products with economic values and better purity be produced, but also the three wastes are hardly discharged to cause pollution, and a semi-finished product of detergent can even be recycled for dissolving raw materials. The method disclosed by the invention not only has the advantage of simple production process and equipment and low cost, but also can be used for effectively treating the environment pollution caused by the salting-out master liquid generated when the zinc powder method is used for preparing the sodium hydrosulfite, and is beneficial to creation of considerable economic benefits at the same time.
Description
Technical field
The invention belongs to the technical field of inorganic chemical industry industry comprehensive administration of three wastes and utilization, particularly a kind of salting-out mother liquor that is equipped with in the vat powder to be produced with the zinc powder legal system prepares the method for sodium sulphite and bariumchloride coproduction powder barium salt.
Technical background
The zinc powder legal system is equipped with vat powder (Na
2S
2O
42H
2O, V-Brite B) be in zinc suspension liquid, to feed sulfurous gas earlier, again with sodium hydroxide carry out metathesis, filter, saltout, dewater, the dry and product that makes.Its important use is to do printing and dyeing reductive agent, association with pulp bleaching agent etc.This method produces a large amount of salting-out mother liquors in salting-out process, one ton of vat powder of average every production just can produce 7～8 cubic metres mother liquor.An enterprise that produces 5000 tons of vat powders per year discharges mother liquor and can reach 3500～4000 cubic metres, not only severe contamination environment, and caused a large amount of losses of resource.Therefore, how fully utilizing salting-out mother liquor, is the research topic of vat powder enterprise-essential.
The staple of salting-out mother liquor is sodium-chlor, S-WAT, sodium hydroxide, sodium hyposulfate and sodium sulfate etc.; Because the technologic difference of each enterprise production, the composition of salting-out mother liquor also has certain difference, and its main chemical compositions is roughly following: sodium chloride content is 240～270 grams per liters; S-WAT content is 40～50 grams per liters; Sodium hydrate content is 35～45 grams per liters, and the SODIUM HYDROSULPHITE sodium content is 13～21 grams per liters, and sodium sulphate content is 5～10 grams per liters.
The method of comprehensive utilization of China's zinc powder method salting-out mother liquor is a lot of at present, has hydrochloric acid synthetic method, direct absorption method, three to steam two and freezes the method for washing, sulfurous gas neutralisation and improvement sulfurous gas neutralisation etc.Wherein the hydrochloric acid neutralisation is the method that technology is simple, investment is minimum with direct absorption method; But the hydrochloric acid neutralisation need consume a large amount of hydrochloric acid, and the cost that reclaims salt is increased substantially, and the quality that not only reclaims salt is on the low side; And slant acidity; Production to vat powder has certain influence, at the reaction process sulfur dioxide gas of can overflowing, also can cause secondary pollution.
Summary of the invention
The invention provides a kind of not only with low cost, reclaim the salt quality high, be easy to realize and production technique and production unit is simple, prepare the method for sodium sulphite and bariumchloride coproduction powder barium salt with the salting-out mother liquor in the zinc powder method; This method can not only be produced more purified sodium sulphite, bariumchloride and powder barium salt, does not almost have the three wastes to discharge simultaneously and pollutes, and just half-finished washings also can recycle dissolving raw material at last.
In order to reach above-mentioned purpose, technical scheme of the present invention is:
Prepare the method for sodium sulphite and bariumchloride coproduction powder barium salt with the salting-out mother liquor in the zinc powder method, comprise being prepared as follows step:
Steps A, salting-out mother liquor that is produced in the zinc powder method and barium sulfide solution are put in the corrosion-resistant reactor according to the mass ratio 1: 0.95～1.58 of pure substance, do not stopped to stir; Reaction generates the mixing solutions of sodium sulphite, bariumchloride, barium sulfite and barium hyposulflte; Pure S-WAT, V-Brite B and the sodium-chlor that is contained in the salting-out mother liquor that said pure substance refers to react with barium sulphide (being the actual amount of putting into the barium sulphide in the corrosion-resistant reactor, is 0.95～1.58 times of calculating according to pure S-WAT, V-Brite B and sodium-chlor sum).The stirring reaction time is indefinite, and it is fixed to come according to the amount of actual treatment salting-out mother liquor.
Step B, the mixing solutions of gained in the steps A is filtered with strainer;
Step C, with the filter cake of gained among the step B, wash drying and drying and crushing with first washing and spin-drying machine, the first drying and crushing machine earlier, carry out the classification selection by winnowing with classification winnowing machine again, obtain powder barium sulfite and barium hyposulflte after the selection by winnowing respectively;
Step D, gained powder barium sulfite among the step C handy first wrapper of checking the weight is checked the weight and is packaged to be powder barium sulfite product, gained powder barium hyposulflte handy second wrapper of checking the weight is checked the weight and is packaged to be powder and connects the barium sulfite product;
Step e, sodium sulphite, the bariumchloride of gained among the step B are filtrated with behind the fractional distillation device fractional distillation; Again respectively successively with first cooling tower, second washing and spin-drying machine, the second drying and crushing machine, the 3rd wrapper of checking the weight, second cooling tower, the 3rd washing and spin-drying machine, the 3rd drying and crushing machine, the 4th check the weight that wrapper is carried out crystallisation by cooling, washing and spin-drying machine, drying and crushing and the packing of checking the weight after obtain sodium sulfide crystal product and bariumchloride crystal product.
The present invention adopts barium sulphide to handle the salting-out mother liquor that the zinc powder legal system is equipped with in the vat powder to be produced, can not only produce economic worth, more purified sodium sulphite, bariumchloride, powder barium sulfite and powder barium hyposulfate product; And almost do not have the three wastes to discharge pollution, just be that the work in-process washings also can recycle dissolving raw material.This method not only production technique and equipment thereof is simple, with low cost, and effectively administered the pollution to environment of salting-out mother liquor that the zinc powder legal system is equipped with in the vat powder to be produced, created considerable economic simultaneously.
Its chemical equation is:
2NaCl+BaS＝＝＝＝Na
2S+BaCl
2
Na
2SO
3+BaS＝＝＝＝Na
2S+BaSO
3
Na
2S
2O
4+BaS＝＝＝＝Na
2S+BaS
2O
4
Description of drawings
Fig. 1 is the process flow diagram for preparing the method for sodium sulphite and bariumchloride coproduction powder barium salt with the salting-out mother liquor in the zinc powder method,
Wherein:
The 1-corrosion-resistant reactor, 2-strainer, 3-first washing and spin-drying machine, the 4-first drying and crushing machine; 5-classification winnowing machine, 6-first wrapper of checking the weight, 7-powder barium sulfite product, 8-second wrapper of checking the weight; 9-powder barium hyposulflte product, 10-fractional distillation device, 11-first cooling tower, 12-second washing and spin-drying machine; The 13-second drying and crushing machine, 14-the 3rd wrapper of checking the weight, 15-second cooling tower, 16-the 3rd washing and spin-drying machine; 17-the 3rd drying and crushing machine, 18-the 4th wrapper of checking the weight, 19-sodium sulfide crystal product, 20-bariumchloride crystal product.
Concrete embodiment
Embodiment 1
Prepare the method for sodium sulphite and bariumchloride coproduction powder barium salt with the salting-out mother liquor in the zinc powder method, comprise being prepared as follows step:
Steps A, will use salting-out mother liquor in the zinc powder method to put into 1 li of corrosion-resistant reactor with barium sulfide solution at 1: 0.95 according to the mass ratio of pure substance for 1000 liters (wherein to contain S-WAT 40Kg, V-Brite B 20Kg, sodium-chlor 250Kg; Mass ratio according to mass ratio 1: 0.95, sodium-chlor and the barium sulphide of mass ratio 1: 0.95, V-Brite B and the barium sulphide of S-WAT and barium sulphide calculates at 1: 0.95 respectively; Then the barium sulphide of required input is 294.5Kg), do not stop to stir; Reaction generates the mixing solutions of sodium sulphite, bariumchloride, barium sulfite barium hyposulflte;
Step B, the mixing solutions of gained in the steps A is filtered with strainer 2;
Step C, with the filter cake of gained among the step B, wash drying and drying and crushing with first washing and spin-drying machine 3, the first drying and crushing machine 4 earlier, carry out the classification selection by winnowing with classification winnowing machine 5 again, obtain powder barium sulfite, barium hyposulflte after the selection by winnowing respectively;
Step D, the inferior barium sulphide handy first of gained powder among the step C wrapper 6 of checking the weight is checked the weight and is packaged to be 48.76Kg powder barium sulfite product 7; Gained powder barium hyposulflte handy second wrapper 8 of checking the weight is checked the weight and is packaged to be 29.77Kg powder barium hyposulflte product 9
Step e, sodium sulphite, the bariumchloride of gained among the step B are filtrated with behind fractional distillation device 10 fractional distillations; Check the weight with first cooling tower 11, second washing and spin-drying machine 12, the second drying and crushing machine the 13, the 3rd that wrapper 14, the second cooling towers 15, the 3rd washing and spin-drying machine 16, the 3rd drying and crushing machine the 17, the 4th check the weight that wrapper 18 is carried out crystallisation by cooling, washing and spin-drying machine, drying and crushing successively respectively again and the packing of checking the weight after obtain 131.77Kg sodium sulfide crystal product 19 and 276.59Kg bariumchloride crystal product 20.
Embodiment 2
Prepare the method for sodium sulphite and bariumchloride coproduction powder barium salt with the salting-out mother liquor in the zinc powder method, comprise being prepared as follows step:
Steps A, will use salting-out mother liquor in the zinc powder method to put into 1 li of corrosion-resistant reactor with barium sulfide solution at 1: 1.58 according to the mass ratio of pure substance for 1000 liters (wherein to contain S-WAT 40Kg, V-Brite B 20Kg, sodium-chlor 250Kg; Mass ratio according to mass ratio 1: 1.58, sodium-chlor and the barium sulphide of mass ratio 1: 1.58, V-Brite B and the barium sulphide of S-WAT and barium sulphide calculates at 1: 1.58 respectively; Then the barium sulphide of required input is 489.8Kg), do not stop to stir; Reaction generates the mixing solutions of sodium sulphite, bariumchloride, barium sulfite barium hyposulflte;
Step B, the mixing solutions of gained in the steps A is filtered with strainer 2;
Step C, with the filter cake of gained among the step B, wash drying and drying and crushing with first washing and spin-drying machine 3, the first drying and crushing machine 4 earlier, carry out the classification selection by winnowing with classification winnowing machine 5 again, obtain powder barium sulfite, barium hyposulflte after the selection by winnowing respectively;
Step D, the inferior barium sulphide handy first of gained powder among the step C wrapper 6 of checking the weight is checked the weight and is packaged to be 68.96Kg powder barium sulfite product 7; Gained powder barium hyposulflte handy second wrapper 8 of checking the weight is checked the weight and is packaged to be 30.47Kg powder barium hyposulflte product 9
Step e, sodium sulphite, the bariumchloride of gained among the step B are filtrated with behind fractional distillation device 10 fractional distillations; Check the weight with first cooling tower 11, second washing and spin-drying machine 12, the second drying and crushing machine the 13, the 3rd that wrapper 14, the second cooling towers 15, the 3rd washing and spin-drying machine 16, the 3rd drying and crushing machine the 17, the 4th check the weight that wrapper 18 is carried out crystallisation by cooling, washing and spin-drying machine, drying and crushing successively respectively again and the packing of checking the weight after obtain 200.67Kg sodium sulfide crystal product 19 and 445.32Kg bariumchloride crystal product 20.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting practical range of the present invention, so all equivalences of being done with described characteristic of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
Claims (2)
1. prepare the method for sodium sulphite and bariumchloride coproduction powder barium salt with the salting-out mother liquor in the zinc powder method, it is characterized in that: comprise being prepared as follows step:
Steps A, salting-out mother liquor that is produced in the zinc powder method and barium sulfide solution are put in the corrosion-resistant reactor according to the mass ratio 1: 0.95～1.58 of pure substance, do not stopped to stir; Reaction generates the mixing solutions of sodium sulphite, bariumchloride, barium sulfite and barium hyposulflte;
Step B, the mixing solutions of gained in the steps A is filtered with strainer;
Step C, with the filter cake of gained among the step B, wash drying and drying and crushing with first washing and spin-drying machine, the first drying and crushing machine earlier, carry out the classification selection by winnowing with classification winnowing machine again, obtain powder barium sulfite and barium hyposulflte after the selection by winnowing respectively;
Step D, gained powder barium sulfite among the step C handy first wrapper of checking the weight is checked the weight and is packaged to be powder barium sulfite product, gained powder barium hyposulflte handy second wrapper of checking the weight is checked the weight and is packaged to be powder barium hyposulflte product;
Step e, sodium sulphite, the bariumchloride of gained among the step B are filtrated with behind the fractional distillation device fractional distillation; Again respectively successively with first cooling tower, second washing and spin-drying machine, the second drying and crushing machine, the 3rd wrapper of checking the weight, second cooling tower, the 3rd washing and spin-drying machine, the 3rd drying and crushing machine, the 4th check the weight that wrapper is carried out crystallisation by cooling, washing and spin-drying machine, drying and crushing and the packing of checking the weight after obtain sodium sulfide crystal product and bariumchloride crystal product.
2. prepare the method for sodium sulphite and bariumchloride coproduction powder barium salt according to the salting-out mother liquor described in the claim 1, it is characterized in that: contained pure sodium chloride, V-Brite B and S-WAT in the salting-out mother liquor that pure substance described in the steps A refers to react with barium sulphide with in the zinc powder method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110142069A CN102328911A (en) | 2011-05-30 | 2011-05-30 | Method for preparing sodium sulfide and barium chloride with cogeneration of powdery barium salt by using salting-out master liquid generated in zinc powder method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110142069A CN102328911A (en) | 2011-05-30 | 2011-05-30 | Method for preparing sodium sulfide and barium chloride with cogeneration of powdery barium salt by using salting-out master liquid generated in zinc powder method |
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| Publication Number | Publication Date |
|---|---|
| CN102328911A true CN102328911A (en) | 2012-01-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110142069A Pending CN102328911A (en) | 2011-05-30 | 2011-05-30 | Method for preparing sodium sulfide and barium chloride with cogeneration of powdery barium salt by using salting-out master liquid generated in zinc powder method |
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|---|---|
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2011
- 2011-05-30 CN CN201110142069A patent/CN102328911A/en active Pending
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Application publication date: 20120125 |