CN102180452A - Method for producing manganese phosphate as well as sodium sulfate and ammonium phosphate with manganese-containing waste liquid generated in production of hydroquinone - Google Patents
Method for producing manganese phosphate as well as sodium sulfate and ammonium phosphate with manganese-containing waste liquid generated in production of hydroquinone Download PDFInfo
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- CN102180452A CN102180452A CN2010106160561A CN201010616056A CN102180452A CN 102180452 A CN102180452 A CN 102180452A CN 2010106160561 A CN2010106160561 A CN 2010106160561A CN 201010616056 A CN201010616056 A CN 201010616056A CN 102180452 A CN102180452 A CN 102180452A
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Abstract
The invention belongs to the technical field of utilization of manganese-containing waste liquid generated in the production of hydroquinone and particularly relates to a method for producing manganese phosphate as well as sodium sulfate and ammonium phosphate with manganese-containing waste liquid generated in the production of hydroquinone. The method mainly comprises the following steps: filtering waste liquid generated in the production of the hydroquinone with a filter to obtain a filtrate; distilling and filtering the obtained filtrate; deeply processing filter cakes to obtain the manganese phosphate; and performing reduced pressure distillation to the filtrate, and then performing deep-processing to obtain the sodium sulfate and the ammonium phosphate. The method has the advantages that the waste liquid can be fully utilized, thereby reducing the pollution of the waste liquid to the environment; and the valuable manganese phosphate as well as the sodium sulfate and the ammonium phosphate products can be produced, so that the method not only has remarkable social and economical benefits, but also is simple in process and production equipment and is a more practical processing and utilization method.
Description
Technical field
The present invention relates to produce the technical field that contains the manganese waste water utilization that Resorcinol produces, particularly a kind of with producing the method that the manganese waste liquid is made manganous phosphate co-producing sodium sulfate and ammonium phosphate that contains that Resorcinol produced.
Technical background
Resorcinol is important organic intermediate, and China has also dropped into suitability for industrialized production in the development seventies in 20th century.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 contains manganese waste liquid the inside of Resorcinol 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%.At present domestic factories' utilizations contain the manganese waste liquid and produce crystal manganous sulfate or common phosphoric acid salt, and high-purity phosphoric acid manganese etc.High-purity phosphoric acid manganese is 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 phosphoric acid manganese mainly is as soft magnet oxygen magneticsubstance at present, is that raw material is produced with electrolytic manganese or manganous sulfate, ammonium hydrogen phosphate etc. generally.But do not have a kind of at present with producing the relevant report that the manganese waste liquid is made the method for manganous phosphate co-producing sodium sulfate and ammonium phosphate that contains that Resorcinol produced yet.
Summary of the invention
The invention provides that a kind of this method not only technology is simple with producing the method that the manganese waste liquid is made manganous phosphate co-producing sodium sulfate and ammonium phosphate that contains that Resorcinol produced, and can also make multiple value product when can effectively dispose waste liquid.
To achieve the above object, technical scheme of the present invention is:
A kind of with producing the method that the manganese waste liquid is made manganous phosphate co-producing sodium sulfate and ammonium phosphate that contains that Resorcinol produced, comprise being prepared as follows step:
Steps A, will produce the waste liquid that Resorcinol produces and carry out suction filtration with the suction filtration machine;
Step B, suction filtration gained simple substance residual filter cake in the steps A is used to develop other products;
Step C, suction filtration gained filtrate in the steps A is transferred in the reactor, drops into sodium radio-phosphate,P-32 solution simultaneously and react, the mass ratio between filtrate and the sodium radio-phosphate,P-32 solution is 1: 0.55～0.95; Reaction generates the mixture I of manganous phosphate and sodium sulfate and ammonium phosphate;
Step D, the mixture I of gained among the step C is filtered with strainer;
Step e, with filter among the step D gained filter cake through wash drying, crushing packing becomes the manganous phosphate product;
Step F, with the clarifying filtrate of sulphur of gained among the step D through underpressure distillation, gradient cooling, crystallization, obtain sodium sulfate crystal and ammonium phosphate crystal respectively;
Step G, with step F gained sodium sulfate crystal through wash drying, crushing packing becomes the sodium sulfate product;
Step H, with step F gained ammonium phosphate crystal through wash drying, crushing packing becomes the ammonium phosphate product.
The present invention carries out suction filtration with the waste liquid that Resorcinol produced with the suction filtration machine earlier, obtains filtrate and carries out distillating filtering, and the filter cake deep processing obtains the manganous phosphate product; Further respectively deep processing obtained sodium sulfate and ammonium phosphate product respectively after filtrate was carried out underpressure distillation again; The present invention can as clean as a pennyly gulp down waste liquid, alleviates the pollution of waste liquid to environment; Can make valuable manganous phosphate, sodium sulfate and ammonium phosphate product again, not only have remarkable social benefit and economic benefit, and technology and production unit are simple, be a kind of relatively actual processing and utilize method.
Its chemical equation is:
3MnSO
4+2Na
3PO
4＝＝＝＝＝Mn
3(PO
4)
2+3Na
2SO
4
3(NH
4)
2SO
4+2Na
3PO
4＝＝＝＝＝2(NH
4)
3PO
4+3Na
2SO
4
3H
2SO
4+2Na
3PO
4＝＝＝＝＝3Na
2SO
4+H
3PO
4
Concrete embodiment
Embodiment 1
A kind of with producing the method that the manganese waste liquid is made manganous phosphate co-producing sodium sulfate and ammonium phosphate that contains that Resorcinol produced, comprise being prepared as follows step:
Steps A, will produce the 1000kg waste liquid (wherein, comprising the 120kg manganous sulfate, 15kg ammonium sulfate and 20kg sulfuric acid) that Resorcinol produces and carry out suction filtration with the suction filtration machine;
Step B, suction filtration gained simple substance residual filter cake in the steps A is used to develop other products;
Step C, suction filtration gained filtrate in the steps A is transferred in the reactor, drops into sodium radio-phosphate,P-32 solution simultaneously and react, the mass ratio between filtrate and the sodium radio-phosphate,P-32 solution is 1: 0.55; Reaction generates the mixture I of manganous phosphate and sodium sulfate and ammonium phosphate;
Step D, the mixture I of gained among the step C is filtered with strainer;
Step e, with filter among the step D gained filter cake through wash drying, crushing packing becomes 81.41kg manganous phosphate product;
Step F, with the clarifying filtrate of sulphur of gained among the step D through underpressure distillation, gradient cooling, crystallization, obtain sodium sulfate crystal and ammonium phosphate crystal respectively;
Step G, with step F gained sodium sulfate crystal through wash drying, crushing packing becomes 110.75kg sodium sulfate product;
Step H, with step F gained ammonium phosphate crystal through wash drying, crushing packing becomes 6.59kg ammonium phosphate product.
Embodiment 2
A kind of with producing the method that the manganese waste liquid is made manganous phosphate co-producing sodium sulfate and ammonium phosphate that contains that Resorcinol produced, comprise being prepared as follows step:
Steps A, will produce the 1000kg waste liquid (wherein, comprising the 120kg manganous sulfate, 15kg ammonium sulfate and 20kg sulfuric acid) that Resorcinol produces and carry out suction filtration with the suction filtration machine;
Step B, suction filtration gained simple substance residual filter cake in the steps A is used to develop other products;
Step C, suction filtration gained filtrate in the steps A is transferred in the reactor, drops into sodium radio-phosphate,P-32 solution simultaneously and react, the mass ratio between filtrate and the sodium radio-phosphate,P-32 solution is 1: 0.75; Reaction generates the mixture I of manganous phosphate and sodium sulfate and ammonium phosphate;
Step D, the mixture I of gained among the step C is filtered with strainer;
Step e, with filter among the step D gained filter cake through wash drying, crushing packing becomes 97.38kg manganous phosphate product;
Step F, with the clarifying filtrate of sulphur of gained among the step D through underpressure distillation, gradient cooling, crystallization, obtain sodium sulfate crystal and ammonium phosphate crystal respectively;
Step G, with step F gained sodium sulfate crystal through wash drying, crushing packing becomes 151.02kg sodium sulfate product;
Step H, with step F gained ammonium phosphate crystal through wash drying, crushing packing becomes 8.99kg ammonium phosphate product.
Embodiment 3
A kind of with producing the method that the manganese waste liquid is made manganous phosphate co-producing sodium sulfate and ammonium phosphate that contains that Resorcinol produced, comprise being prepared as follows step:
Steps A, will produce the 1000kg waste liquid (wherein, comprising the 120kg manganous sulfate, 15kg ammonium sulfate and 20kg sulfuric acid) that Resorcinol produces and carry out suction filtration with the suction filtration machine;
Step B, suction filtration gained simple substance residual filter cake in the steps A is used to develop other products;
Step C, suction filtration gained filtrate in the steps A is transferred in the reactor, drops into sodium radio-phosphate,P-32 solution simultaneously and react, the mass ratio between filtrate and the sodium radio-phosphate,P-32 solution is 1: 0.95; Reaction generates the mixture I of manganous phosphate and sodium sulfate and ammonium phosphate;
Step D, the mixture I of gained among the step C is filtered with strainer;
Step e, with filter among the step D gained filter cake through wash drying, crushing packing becomes 123.35kg manganous phosphate product;
Step F, with the clarifying filtrate of sulphur of gained among the step D through underpressure distillation, gradient cooling, crystallization, obtain sodium sulfate crystal and ammonium phosphate crystal respectively;
Step G, with step F gained sodium sulfate crystal through wash drying, crushing packing becomes 191.28kg sodium sulfate product;
Step H, with step F gained ammonium phosphate crystal through wash drying, crushing packing becomes 11.38kg ammonium phosphate product.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting the scope of the present invention, so all equivalences of being done with described feature of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
Claims (1)
1. one kind with producing the method that the manganese waste liquid is made manganous phosphate co-producing sodium sulfate and ammonium phosphate that contains that Resorcinol produced, and it is characterized in that, comprises being prepared as follows step:
Steps A, will produce the waste liquid that Resorcinol produces and carry out suction filtration with the suction filtration machine;
Step B, suction filtration gained simple substance residual filter cake in the steps A is used to develop other products;
Step C, suction filtration gained filtrate in the steps A is transferred in the reactor, drops into sodium radio-phosphate,P-32 solution simultaneously and react, the mass ratio between filtrate and the sodium radio-phosphate,P-32 solution is 1: 0.55～0.95; Reaction generates the mixture I of manganous phosphate and sodium sulfate and ammonium phosphate;
Step D, the mixture I of gained among the step C is filtered with strainer;
Step e, with filter among the step D gained filter cake through wash drying, crushing packing becomes the manganous phosphate product;
Step F, with the clarifying filtrate of sulphur of gained among the step D through underpressure distillation, gradient cooling, crystallization, obtain sodium sulfate crystal and ammonium phosphate crystal respectively;
Step G, with step F gained sodium sulfate crystal through wash drying, crushing packing becomes the sodium sulfate product;
Step H, with step F gained ammonium phosphate crystal through wash drying, crushing packing becomes the ammonium phosphate product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106160561A CN102180452A (en) | 2010-12-30 | 2010-12-30 | Method for producing manganese phosphate as well as sodium sulfate and ammonium phosphate with manganese-containing waste liquid generated in production of hydroquinone |
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| CN2010106160561A CN102180452A (en) | 2010-12-30 | 2010-12-30 | Method for producing manganese phosphate as well as sodium sulfate and ammonium phosphate with manganese-containing waste liquid generated in production of hydroquinone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381387A (en) * | 2016-09-09 | 2017-02-08 | 北京科技大学 | Method for preparing high-purity manganese phosphate from low-grade rhodochrosite leaching liquid |
-
2010
- 2010-12-30 CN CN2010106160561A patent/CN102180452A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106381387A (en) * | 2016-09-09 | 2017-02-08 | 北京科技大学 | Method for preparing high-purity manganese phosphate from low-grade rhodochrosite leaching liquid |
| CN106381387B (en) * | 2016-09-09 | 2018-04-13 | 北京科技大学 | A kind of method that high-purity phosphoric acid manganese is prepared from low grade rhodochrosite leachate |
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Application publication date: 20110914 |