CN102115144A - Method for preparing mixed chlorides and calcium sulfate by using manganese-containing waste liquid - Google Patents
Method for preparing mixed chlorides and calcium sulfate by using manganese-containing waste liquid Download PDFInfo
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- CN102115144A CN102115144A CN2010106156814A CN201010615681A CN102115144A CN 102115144 A CN102115144 A CN 102115144A CN 2010106156814 A CN2010106156814 A CN 2010106156814A CN 201010615681 A CN201010615681 A CN 201010615681A CN 102115144 A CN102115144 A CN 102115144A
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- chloride
- sulfate
- calcium sulfate
- waste liquid
- calcium
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Abstract
The invention provides a method for preparing mixed chlorides and calcium sulfate by using a manganese-containing waste liquid. The method comprises the following steps: filtering the manganese-containing waste liquid obtained by producing p-dihydroxybenzene so as to obtain a clear filtrate containing manganese sulfate, ammonium sulfate and sulfuric acid and a filter cake containing single substance residues; reacting the filter cake containing single substance residues with excess sulfuric acid so as to obtain a solution containing calcium sulfate, magnesium sulfate, zinc sulfate, sodium sulfate, aluminum sulfate, cadmium sulfate and nickel sulfate; mixing and reacting the solution with a calcium chloride solution so as to obtain a mixed solution of chlorides and calcium sulfate; filtering the obtained mixed solution of chlorides and calcium sulfate so as to obtain a calcium sulfate filter cake and chloride filtrate; washing, drying and smashing the calcium sulfate filter cake so as to obtain the calcium sulfate product; and distilling the chloride filtrate under reduced pressure, and then carrying out cooling crystallization so as to obtain the mixed chloride product.
Description
Technical field
The present invention relates to contain the technical field of the improvement and the utilization of manganese waste liquid, especially a kind of usefulness contains the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, and the described manganese waste liquid that contains contains the manganese waste liquid for producing the Resorcinol gained.
Background technology
Resorcinol is important organic intermediate, and China is in the development seventies in 20th century and dropped into suitability for industrialized production.Advantages such as at present domestic mainly taking used aniline-Manganse Dioxide explained hereafter Resorcinol, and this technology is compared with external phenol-hydrogen peroxide process, has the product purity height, and impurity is few.But its shortcoming is that the quantity discharged of waste liquid is big.Under the common state, one ton of Resorcinol of every production has 40 tons of Mn-bearing waste waters approximately.The chemical composition that production Resorcinol gained contains manganese waste liquid the inside is the content 11-12% of manganous sulfate, and ammonium sulfate content is 1.4-1.6%, and sulfuric acid content is 1.8-2.2%, simple substance element residue 5-6%, and the simple substance element is: calcium, magnesium, zinc, sodium, aluminium, cadmium and nickel.
At present domestic factories' utilizations contain the manganese waste liquid and produce crystal manganous sulfate or common carbonate, and high-purity manganese carbonate etc.High-purity manganese carbonate is an ideal high performance strong magneticsubstance, is the main raw material of the manganese-silicon that developed rapidly modern age, mangal, high-performance manganese dioxide product.High-purity manganese carbonate mainly is as soft magnet oxygen magneticsubstance at present, is that raw material is produced with electrolytic manganese or manganous sulfate, bicarbonate of ammonia etc. generally.The utilization of domestic existing factory contains the manganese waste liquid and produces the manganous sulfate crystal through a series of purification process, and carry out replacement(metathesis)reaction with bicarbonate of ammonia again and produce high-purity manganese carbonate,
Yet, but be not used with other chemical ingredients in the Resorcinol, thereby, resource wasted.
Summary of the invention
The chemical composition that production Resorcinol gained contains the manganese waste liquid is the content 11-12% of manganous sulfate, and ammonium sulfate content is 1.4-1.6%, and sulfuric acid content is 1.8-2.2%, simple substance element residue 5-6%, and the simple substance element is: calcium, magnesium, zinc, sodium, aluminium, cadmium and nickel.For it is fully utilized, the invention provides a kind of usefulness and contain the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, the described manganese waste liquid that contains contains the manganese waste liquid for producing the Resorcinol gained, this method is simple to operate, facility investment is few, will produce the Resorcinol gained and contain the comprehensive utilization of manganese waste liquid, turns waste into wealth, eliminated and contained of the pollution of manganese waste liquid, improved economic benefit of enterprises environment.
Technical scheme of the present invention is as follows: a kind of usefulness contains the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, and the described manganese waste liquid that contains contains the manganese waste liquid for producing the Resorcinol gained, comprises following concrete steps:
Steps A: will produce the Resorcinol gained and contain the filter cake that obtains clarifying sulfur acid manganese, ammonium sulfate, vitriolic filtrate behind the manganese waste liquid suction filtration and contain the simple substance residue, described filtrate is developed other products separately;
Step B: described filter cake and the excess sulfuric acid reaction that contains the simple substance residue, obtain sulfur acid calcium, sal epsom, zinc sulfate, sodium sulfate, the solution of Tai-Ace S 150, Cadmium Sulphate and single nickel salt, then mix with calcium chloride solution again, and to make the ratio of molar content sum and the molar content of calcium chloride of the material of vitriol in the solution be 1: 1-1.5 obtains containing the muriate of magnesium chloride, sodium-chlor, zinc chloride, aluminum chloride, Cadmium chloride fine powder and nickelous chloride and the mixing solutions of calcium sulfate;
Step C: with the mixing solutions of step B gained muriate and calcium sulfate after filtration, obtain calcium sulfate filter cake and muriate filtrate;
Step D: the calcium sulfate filter cake obtains the calcium sulfate product through washing, drying, pulverizing;
Step e: muriate filtrate through underpressure distillation, crystallisation by cooling, obtain containing the mixed chloride product of magnesium chloride, sodium-chlor, aluminum chloride, zinc chloride, Cadmium chloride fine powder, nickelous chloride.
Usefulness of the present invention contains the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, its chemical equation:
MgSO
4+CaCl
2＝＝＝＝＝MgCl
2+CaSO
4
Na
2SO
4+CaCl
2＝＝＝＝＝2NaCl+CaSO
4
ZnSO
4+CaCl
2＝＝＝＝＝ZnCl
2+CaSO
4
Al
2(SO
4)
3+3CaCl
2＝＝＝＝＝2AlCl
3+3CaSO
4
CdSO
4+CaCl
2＝＝＝＝＝CdCl
2+CaSO
4
NiSO
4+CaCl
2＝＝＝＝＝NiCl
2+CaSO
4
Beneficial effect of the present invention is: usefulness of the present invention contains the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, the described manganese waste liquid that contains contains the manganese waste liquid for producing the Resorcinol gained, this method is simple to operate, facility investment is few, to produce the Resorcinol gained and contain the comprehensive utilization of manganese waste liquid, turn waste into wealth, eliminated and contain of the pollution of manganese waste liquid, improved economic benefit of enterprises environment.
Embodiment
Embodiment 1:
A kind of usefulness contains the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, and the described manganese waste liquid that contains contains the manganese waste liquid for producing the Resorcinol gained, comprises following concrete steps:
Steps A: 500kg is produced the Resorcinol gained contain the filter cake that obtains clarifying sulfur acid manganese, ammonium sulfate, vitriolic filtrate behind the manganese waste liquid suction filtration and contain the simple substance residue, described filtrate is developed other products separately;
Step B: described filter cake and the excess sulfuric acid reaction that contains the simple substance residue, obtain sulfur acid calcium, sal epsom, zinc sulfate, sodium sulfate, the solution of Tai-Ace S 150, Cadmium Sulphate and single nickel salt, then mix with calcium chloride solution again, and to make the ratio of molar content sum and the molar content of calcium chloride of the material of vitriol in the solution be 1: 1, obtains containing the muriate of magnesium chloride, sodium-chlor, zinc chloride, aluminum chloride, Cadmium chloride fine powder and nickelous chloride and the mixing solutions of calcium sulfate;
Step C: with the mixing solutions of step B gained muriate and calcium sulfate after filtration, obtain calcium sulfate filter cake and muriate filtrate;
Step D: the calcium sulfate filter cake obtains the calcium sulfate product through washing, drying, pulverizing;
Step e: muriate filtrate through underpressure distillation, crystallisation by cooling, obtain containing the mixed chloride product of magnesium chloride, sodium-chlor, aluminum chloride, zinc chloride, Cadmium chloride fine powder, nickelous chloride.
Embodiment 2:
A kind of usefulness contains the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, and the described manganese waste liquid that contains contains the manganese waste liquid for producing the Resorcinol gained, comprises following concrete steps:
Steps A: 500kg is produced the Resorcinol gained contain the filter cake that obtains clarifying sulfur acid manganese, ammonium sulfate, vitriolic filtrate behind the manganese waste liquid suction filtration and contain the simple substance residue, described filtrate is developed other products separately;
Step B: described filter cake and the excess sulfuric acid reaction that contains the simple substance residue, obtain sulfur acid calcium, sal epsom, zinc sulfate, sodium sulfate, the solution of Tai-Ace S 150, Cadmium Sulphate and single nickel salt, then mix with calcium chloride solution again, and to make the ratio of molar content sum and the molar content of calcium chloride of the material of vitriol in the solution be 1: 1.5, obtains containing the muriate of magnesium chloride, sodium-chlor, zinc chloride, aluminum chloride, Cadmium chloride fine powder and nickelous chloride and the mixing solutions of calcium sulfate;
Step C: with the mixing solutions of step B gained muriate and calcium sulfate after filtration, obtain calcium sulfate filter cake and muriate filtrate;
Step D: the calcium sulfate filter cake obtains the calcium sulfate product through washing, drying, pulverizing;
Step e: muriate filtrate through underpressure distillation, crystallisation by cooling, obtain containing the mixed chloride product of magnesium chloride, sodium-chlor, aluminum chloride, zinc chloride, Cadmium chloride fine powder, nickelous chloride.
Embodiment 3:
A kind of usefulness contains the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, and the described manganese waste liquid that contains contains the manganese waste liquid for producing the Resorcinol gained, comprises following concrete steps:
Steps A: 500kg is produced the Resorcinol gained contain the filter cake that obtains clarifying sulfur acid manganese, ammonium sulfate, vitriolic filtrate behind the manganese waste liquid suction filtration and contain the simple substance residue, described filtrate is developed other products separately;
Step B: described filter cake and the excess sulfuric acid reaction that contains the simple substance residue, obtain sulfur acid calcium, sal epsom, zinc sulfate, sodium sulfate, the solution of Tai-Ace S 150, Cadmium Sulphate and single nickel salt, then mix with calcium chloride solution again, and to make the ratio of molar content sum and the molar content of calcium chloride of the material of vitriol in the solution be 1: 1.2, obtains containing the muriate of magnesium chloride, sodium-chlor, zinc chloride, aluminum chloride, Cadmium chloride fine powder and nickelous chloride and the mixing solutions of calcium sulfate;
Step C: with the mixing solutions of step B gained muriate and calcium sulfate after filtration, obtain calcium sulfate filter cake and muriate filtrate;
Step D: the calcium sulfate filter cake obtains the calcium sulfate product through washing, drying, pulverizing;
Step e: muriate filtrate through underpressure distillation, crystallisation by cooling, obtain containing the mixed chloride product of magnesium chloride, sodium-chlor, aluminum chloride, zinc chloride, Cadmium chloride fine powder, nickelous chloride.
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 product.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 (1)
1. one kind with containing the method that the manganese waste liquid prepares mixed chloride and calcium sulfate, it is characterized in that, the described manganese waste liquid that contains contains the manganese waste liquid for producing the Resorcinol gained, comprises following concrete steps:
Steps A: will produce the Resorcinol gained and contain the filter cake that obtains clarifying sulfur acid manganese, ammonium sulfate, vitriolic filtrate behind the manganese waste liquid suction filtration and contain the simple substance residue, described filtrate is developed other products separately;
Step B: described filter cake and the excess sulfuric acid reaction that contains the simple substance residue, obtain sulfur acid calcium, sal epsom, zinc sulfate, sodium sulfate, the solution of Tai-Ace S 150, Cadmium Sulphate and single nickel salt, then mix with calcium chloride solution again, and to make the ratio of molar content sum and the molar content of calcium chloride of the material of vitriol in the solution be 1: 1-1.5 obtains containing the muriate of magnesium chloride, sodium-chlor, zinc chloride, aluminum chloride, Cadmium chloride fine powder and nickelous chloride and the mixing solutions of calcium sulfate;
Step C: with the mixing solutions of step B gained muriate and calcium sulfate after filtration, obtain calcium sulfate filter cake and muriate filtrate;
Step D: the calcium sulfate filter cake obtains the calcium sulfate product through washing, drying, pulverizing;
Step e: muriate filtrate through underpressure distillation, crystallisation by cooling, obtain containing the mixed chloride product of magnesium chloride, sodium-chlor, aluminum chloride, zinc chloride, Cadmium chloride fine powder, nickelous chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106156814A CN102115144A (en) | 2010-12-30 | 2010-12-30 | Method for preparing mixed chlorides and calcium sulfate by using manganese-containing waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106156814A CN102115144A (en) | 2010-12-30 | 2010-12-30 | Method for preparing mixed chlorides and calcium sulfate by using manganese-containing waste liquid |
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|---|---|
| CN102115144A true CN102115144A (en) | 2011-07-06 |
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|---|---|---|---|
| CN2010106156814A Pending CN102115144A (en) | 2010-12-30 | 2010-12-30 | Method for preparing mixed chlorides and calcium sulfate by using manganese-containing waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451550A (en) * | 2019-09-04 | 2019-11-15 | 山东海天生物化工有限公司 | One-step method prepares the method and semi-hydrated gypsum of semi-hydrated gypsum co-production Aluminum Chloride Hexahydrate |
-
2010
- 2010-12-30 CN CN2010106156814A patent/CN102115144A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451550A (en) * | 2019-09-04 | 2019-11-15 | 山东海天生物化工有限公司 | One-step method prepares the method and semi-hydrated gypsum of semi-hydrated gypsum co-production Aluminum Chloride Hexahydrate |
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Application publication date: 20110706 |