CN102328948A - Method for preparing caustic soda and barium chloride and coproducing powdery barium salt by using salting-out mother liquor generated in zinc powder method - Google Patents
Method for preparing caustic soda and barium chloride and coproducing powdery barium salt by using salting-out mother liquor generated in zinc powder method Download PDFInfo
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- CN102328948A CN102328948A CN201110142136A CN201110142136A CN102328948A CN 102328948 A CN102328948 A CN 102328948A CN 201110142136 A CN201110142136 A CN 201110142136A CN 201110142136 A CN201110142136 A CN 201110142136A CN 102328948 A CN102328948 A CN 102328948A
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Abstract
The invention belongs to the technical field of treatment and utilization of the three wastes in the chemical industry, and in particular relates to a method for preparing caustic soda and barium chloride and coproducing powdery barium salt by using salting-out mother liquor generated in a zinc powder method. According to the invention, barium hydroxide is used to treat the salting-out mother liquor generated in the preparation of sodium hydrosulfite by using the zinc powder method, thus not only can caustic soda, barium chloride and powdery barium salt products which have economic values and are relatively pure be produced, but also almost no pollution is caused by the emission of the three wastes, and even a semi-finished cleaning solution can also be recovered and utilized to dissolve raw materials. The method has the advantages of simple production process, simple equipment and low cost; and by using the method, the environmental pollution of the salting-out mother liquor, which is generated in the preparation of sodium hydrosulfite by using the zinc powder method, can be effectively treated, and simultaneously, considerable economic benefits are created.
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 caustic soda and bariumchloride coproduction powder barium salt.
Technical background
Zinc powder method 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, V-Brite B 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 salting-out mother liquor is a lot of in China's zinc powder method 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 caustic soda 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 caustic soda, 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 caustic soda 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 hydroxide solution are put in the corrosion-resistant reactor according to the mass ratio 1: 0.95～1.60 of pure substance, do not stopped to stir; Reaction generates the mixing solutions of sodium hydroxide, bariumchloride, permanent white, barium sulfite and barium hyposulflte; Pure S-WAT, sodium-chlor, V-Brite B and the sodium sulfate that is contained in the salting-out mother liquor that said pure substance refers to react with hydrated barta (being the actual amount of putting into the hydrated barta in the corrosion-resistant reactor, is 0.95～1.60 times of calculating according to pure S-WAT, sodium sulfate, 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 with first washing and spin-drying machine, the first drying and crushing machine earlier and dry and drying and crushing; Carry out the classification selection by winnowing with classification winnowing machine again, obtain powder barium sulfite, barium hyposulflte and permanent white 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; Gained powder permanent white the 3rd wrapper of checking the weight is checked the weight and is packaged to be the powder barium sulfate product;
Step e, the filtrating of gained among the step B is carried out purifying treatment (mainly being to neutralize hydrated barta superfluous in the steps A) with a little sodium-chlor earlier; Use fractional distillation device fractional distillation again; Then respectively successively with first cooling tower, second washing and spin-drying machine, the second drying and crushing machine, the 4th wrapper of checking the weight, second cooling tower, the 3rd washing and spin-drying machine, the 3rd drying and crushing machine, the 5th wrapper of checking the weight carries out crystallisation by cooling, washing and spin-drying machine, drying and crushing and checks the weight obtaining caustic soda crystal product and bariumchloride crystal product after packing.
Wherein, contained pure sodium chloride, sodium sulfate, V-Brite B, S-WAT and sodium sulfate in the salting-out mother liquor that refers to react with hydrated barta of pure substance described in the steps A.
The present invention adopts hydrated barta 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 caustic soda, bariumchloride and powder barium salt product (comprising powder permanent white, powder barium sulfite and powder barium hyposulfate); 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+Ba(OH)
4＝＝＝＝2NaOH+BaCl
Na
2SO
3+Ba(OH)
4＝＝＝＝2NaOH+BaSO
3
Na
2S
2O
4+Ba(OH)
4＝＝＝＝2NaOH+BaS
2O
4
Na
2SO
4+Ba(OH)
4＝＝＝＝2NaOH+BaSO
4
Description of drawings
Fig. 1 is the process flow diagram for preparing the method for caustic soda 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-the 3rd wrapper of checking the weight; 11-powder barium sulfate product, 12-fractional distillation device, 13-the-cooling tower, 14-second washing and spin-drying machine; The 15-second drying and crushing machine, 16-the 4th wrapper of checking the weight, 17-second cooling tower, 18-the 3rd washing and spin-drying machine; 19-the 3rd drying and crushing machine, 20-the 5th wrapper of checking the weight, 21-caustic soda crystal product, 22-bariumchloride crystal product.
Concrete embodiment
Embodiment 1
Prepare the method for caustic soda 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 hydroxide solution at 1: 0.95 according to the mass ratio of pure substance for 1000 liters (wherein to contain sodium-chlor 250Kg, S-WAT 40Kg, V-Brite B 20Kg and sodium sulfate 10Kg; Mass ratio according to mass ratio 1: 0.95, sodium sulfate and the hydrated barta of mass ratio 1: 0.95, V-Brite B and the hydrated barta of mass ratio 1: 0.95, S-WAT and the hydrated barta of sodium-chlor and hydrated barta calculates at 1: 0.95 respectively; Then the bariumchloride of required input is 304Kg), do not stop to stir; Reaction generates the mixing solutions of sodium hydroxide, bariumchloride, permanent white, barium sulfite and 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; Earlier wash drying and drying and crushing with first washing and spin-drying machine 3, the first drying and crushing machine 4; Carry out the classification selection by winnowing with classification winnowing machine 5 again, obtain powder barium sulfite, barium hyposulflte and permanent white after the selection by winnowing respectively;
Step D, gained powder barium sulfite among the step C handy first wrapper 6 of checking the weight is checked the weight and is packaged to be 48.22Kg 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 29.43Kg powder barium hyposulflte product 9, and gained powder permanent white the 3rd wrapper 10 of checking the weight is checked the weight and is packaged to be 12.94Kg powder barium sulfate product 11;
Step e, the filtrating of gained among the step B carried out purifying treatment (mainly being to neutralize hydrated barta superfluous in the steps A) with a little sodium-chlor earlier after; Use fractional distillation device 12 fractional distillations again; Then carry out crystallisation by cooling, washing and spin-drying machine, drying and crushing and check the weight obtaining 136.11Kg caustic soda crystal product 21 and 273.46Kg bariumchloride crystal product 22 after packing with first cooling tower 13, second washing and spin-drying machine 14, the second drying and crushing machine the 15, the 4th wrapper 16, the second cooling towers 17, the 3rd washing and spin-drying machine 18, the 3rd drying and crushing machine the 19, the 5th wrapper 20 of checking the weight of checking the weight successively respectively.
Embodiment 2
Prepare the method for caustic soda 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 hydroxide solution at 1: 1.60 according to the mass ratio of pure substance for 1000 liters (wherein to contain sodium-chlor 250Kg, S-WAT 40Kg, V-Brite B 20Kg and sodium sulfate 10Kg; Mass ratio according to mass ratio 1: 1.60, sodium sulfate and the hydrated barta of mass ratio 1: 1.60, V-Brite B and the hydrated barta of mass ratio 1: 1.60, S-WAT and the hydrated barta of sodium-chlor and hydrated barta calculates at 1: 1.60 respectively; Then the hydrated barta of required input is 512Kg), do not stop to stir; Reaction generates the mixing solutions of sodium hydroxide, bariumchloride, permanent white, barium sulfite and 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; Earlier wash drying and drying and crushing with first washing and spin-drying machine 3, the first drying and crushing machine 4; Carry out the classification selection by winnowing with classification winnowing machine 5 again, obtain powder barium sulfite, barium hyposulflte and permanent white after the selection by winnowing respectively;
Step D, gained powder barium sulfite among the step C handy first wrapper 6 of checking the weight is checked the weight and is packaged to be 68.98Kg 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 30.49Kg powder barium hyposulflte product 9, and gained powder permanent white the 3rd wrapper 10 of checking the weight is checked the weight and is packaged to be 16.43Kg powder barium sulfate product 11;
Step e, the filtrating of gained among the step B carried out purifying treatment (mainly being to neutralize hydrated barta superfluous in the steps A) with a little sodium-chlor earlier after; Use fractional distillation device 12 fractional distillations again; Then carry out crystallisation by cooling, washing and spin-drying machine, drying and crushing and check the weight obtaining 211.29Kg caustic soda crystal product 21 and 445.32Kg bariumchloride crystal product 22 after packing with first cooling tower 13, second washing and spin-drying machine 14, the second drying and crushing machine the 15, the 4th wrapper 16, the second cooling towers 17, the 3rd washing and spin-drying machine 18, the 3rd drying and crushing machine the 19, the 5th wrapper 20 of checking the weight of checking the weight successively respectively.
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 (3)
1. prepare the method for caustic soda 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 hydroxide solution are put in the corrosion-resistant reactor according to the mass ratio 1: 0.95～1.60 of pure substance, do not stopped to stir; Reaction generates the mixing solutions of sodium hydroxide, bariumchloride, permanent white, 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 with first washing and spin-drying machine, the first drying and crushing machine earlier and dry and drying and crushing; Carry out the classification selection by winnowing with classification winnowing machine again, obtain powder barium sulfite, barium hyposulflte and permanent white 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; Gained powder permanent white the 3rd wrapper of checking the weight is checked the weight and is packaged to be the powder barium sulfate product;
Step e, the filtrating of gained among the step B is first 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 4th wrapper of checking the weight, second cooling tower, the 3rd washing and spin-drying machine, the 3rd drying and crushing machine, the 5th 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 caustic soda crystal product and bariumchloride crystal product.
2. prepare the method for caustic soda 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, S-WAT and sodium sulfate in the salting-out mother liquor that pure substance described in the steps A refers to react with hydrated barta with in the zinc powder method.
3. prepare the method for caustic soda and bariumchloride coproduction powder barium salt according to the salting-out mother liquor with in the zinc powder method described in the claim 1, it is characterized in that: in the step e, said filtrating is carried out purifying treatment with sodium-chlor earlier before distilling with the fractional distillation device.
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|---|---|---|---|
| CN201110142136A CN102328948A (en) | 2011-05-30 | 2011-05-30 | Method for preparing caustic soda and barium chloride and coproducing powdery barium salt by using salting-out mother liquor generated in zinc powder method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110142136A CN102328948A (en) | 2011-05-30 | 2011-05-30 | Method for preparing caustic soda and barium chloride and coproducing powdery barium salt by using salting-out mother liquor generated in zinc powder method |
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2011
- 2011-05-30 CN CN201110142136A patent/CN102328948A/en active Pending
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Application publication date: 20120125 |