CN101081809B - Method for circulating utilization of reclaimed pyrolusite powder in benzoquinone manufacturing technique - Google Patents
Method for circulating utilization of reclaimed pyrolusite powder in benzoquinone manufacturing technique Download PDFInfo
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- CN101081809B CN101081809B CN2007100524863A CN200710052486A CN101081809B CN 101081809 B CN101081809 B CN 101081809B CN 2007100524863 A CN2007100524863 A CN 2007100524863A CN 200710052486 A CN200710052486 A CN 200710052486A CN 101081809 B CN101081809 B CN 101081809B
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- pyrolusite powder
- para benzoquinone
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Abstract
The process of producing para-benzoquinone with reuse of recovered pyrolusite powder includes: throwing pyrolusite powder and 36 % concentration dilute sulfuric acid solution in the ratio of 1 g to 2-2.5 ml into one oxidizing tank, dropping aniline in the amount of 20 wt% of pyrolusite powder to react, distilling to obtain para-benzoquinone after finishing reaction, separating the residual liquidin a gravitational settler into waste liquid and manganese dioxide dreg, recovering manganese with the waste liquid, separating manganese dioxide powder from manganese dioxide dreg through gravitational settling, and returning the manganese dioxide powder to the oxidizing tank for further para-benzoquinone production. The present invention has high product yield, high pyrolusite powder utilizing rate and high economic benefit.
Description
Technical field
The present invention relates in a kind of pyrolusite powder oxidation Aniline Production para benzoquinone technology to improve the utilization ratio of manganese and the method for para benzoquinone yield, particularly a kind ofly reclaim the method that pyrolusite powder recycles in the para benzoquinone production technique.
Background technology
In the technology that adopts pyrolusite powder oxidation Aniline Production para benzoquinone, though in order to guarantee the yield of para benzoquinone, pyrolusite powder is excessive; The content of its Manganse Dioxide generally between 45-70%, has guaranteed the effecting reaction concentration of oxygenant, but owing to its particle size differs; When participating in oxidizing reaction, become small-particle after its particle is peeled off layer by layer and participate in oxidizing reaction, during reaction end; Still have the part manganese ore to have neither part nor lot in reaction, but this moment, reductive agent aniline can not transform (oxygenant manganese ore powder is not enough, is difficult to continue oxidation aniline) again; The para benzoquinone yield is influenced, and other producer directly will contain the waste sludge discharge of this manganese ore powder, and it is high to cause manganese powder to consume.
Summary of the invention
The object of the invention just provides a kind of method that pyrolusite powder recycles that reclaims in the para benzoquinone production technique; Its employing is reclaimed manganese powder completely with the unreacted that produces behind the pyrolusite powder once oxidation aniline and is returned the input oxidation trough; Because effective manganese content generally between 5-40%, after this reclaims manganese powder through recycle, can promote the raising of the yield of para benzoquinone in the recovery manganese powder; The more important thing is the utilization ratio of the manganese that has improved pyrolusite, have tangible economic benefit.
The objective of the invention is to realize like this: a kind ofly reclaim the method that pyrolusite powder recycles in the para benzoquinone production technique, be 36% dilute sulphuric acid with pyrolusite powder and concentration by 1g: 2ml-2.5ml puts into oxidation trough, drips aniline then and reacts; The dripping quantity of aniline is 20% of a pyrolusite powder amount; Reaction distills out para benzoquinone after finishing, and raffinate gets into gravitational settler; Isolate waste liquid and manganese slag; Waste liquid is used for reclaiming system manganese goods, and the manganese slag goes out manganese powder through gravity settling separation, and manganese powder remakes to raw material and drops in the oxidation trough that para benzoquinone is produced next time.The content of said pyrolusite powder Manganse Dioxide is 45%-70%.Said manganese powder is meant pyrolusite powder after oxidizing reaction, and through the deposition manganese powder that gravity settling separation produces, the content of its Manganse Dioxide is 5%-40%.
Because adopt method of the present invention, so thereby increase the productive rate that concentration of reactants improves resultant through adding excessive manganese powder, improve the utilization ratio of the manganese of pyrolusite, reach the purpose that produces obvious economic benefit.
Description of drawings
Below in conjunction with embodiment and accompanying drawing the present invention is further described.
Fig. 1 is a process flow diagram of the present invention.
Fig. 1 double as Figure of abstract.
Embodiment
Embodiment 1: adding Manganse Dioxide content is 45% pyrolusite powder 600g, 36% dilute sulphuric acid 1350ml in the 2L reactor drum, drips aniline 120g, after reaction finishes; Distill out para benzoquinone, crystallization, the dry para benzoquinone 95g that gets, distillation residue go out waste liquid and manganese slag through gravity settling separation; The about 400g of manganese slag; Analyzing Manganse Dioxide content is 5%, and waste liquid is processed into the manganese goods, gets manganese sulfate product 320g.Adding Manganse Dioxide content is 45% pyrolusite powder 600g, recovery manganese powder 400g, 36% dilute sulphuric acid 1350ml in another 2L reactor drum; Drip aniline 120g, after reaction finishes, distill out para benzoquinone; Crystallization, the dry para benzoquinone 98g that gets; Distillation residue go out waste liquid and manganese slag through gravity settling separation, and waste liquid is processed into the manganese goods, get manganese sulfate product 332g.
Embodiment 2: adding Manganse Dioxide content is 70% pyrolusite powder 600g, 36% dilute sulphuric acid 1350ml in the 2L reactor drum, drips aniline 120g, after reaction finishes; Distill out para benzoquinone, crystallization, the dry para benzoquinone 105g that gets, distillation residue go out waste liquid and manganese slag through gravity settling separation; The about 360g of manganese slag; Analyzing Manganse Dioxide content is 40%, and waste liquid is processed into the manganese goods, gets manganese sulfate product 378g.Adding Manganse Dioxide content is 70% pyrolusite powder 600g, recovery manganese powder 360g, 36% dilute sulphuric acid 1350ml in another 2L reactor drum; Drip aniline 120g, after reaction finishes, distill out para benzoquinone; Crystallization, the dry para benzoquinone 113g that gets; Distillation residue go out waste liquid and manganese slag through gravity settling separation, and waste liquid is processed into the manganese goods, get manganese sulfate product 389g.
Claims (3)
1. one kind is reclaimed the method that pyrolusite powder recycles in the para benzoquinone production technique, it is characterized in that: be 36% dilute sulphuric acid with pyrolusite powder and concentration by 1g: 2ml-2.5ml puts into oxidation trough, drips aniline then and reacts; The dripping quantity of aniline is 20% of a pyrolusite powder amount; Reaction distills out para benzoquinone after finishing, and raffinate gets into gravitational settler; Isolate waste liquid and manganese slag; Waste liquid is used for reclaiming system manganese goods, and the manganese slag goes out manganese powder through gravity settling separation, and manganese powder remakes to raw material and drops in the oxidation trough that para benzoquinone is produced next time.
2. reclaim the method that pyrolusite powder recycles according to a kind of described in claims 1 in the para benzoquinone production technique, it is characterized in that: the content of said pyrolusite powder Manganse Dioxide is 45%-70%.
3. reclaim the method that pyrolusite powder recycles according to a kind of described in claims 1 in the para benzoquinone production technique; It is characterized in that: said manganese powder is meant that pyrolusite powder is after oxidizing reaction; Through the deposition manganese powder that gravity settling separation produces, the content of its Manganse Dioxide is 5%-40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100524863A CN101081809B (en) | 2007-06-15 | 2007-06-15 | Method for circulating utilization of reclaimed pyrolusite powder in benzoquinone manufacturing technique |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100524863A CN101081809B (en) | 2007-06-15 | 2007-06-15 | Method for circulating utilization of reclaimed pyrolusite powder in benzoquinone manufacturing technique |
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| CN101081809A CN101081809A (en) | 2007-12-05 |
| CN101081809B true CN101081809B (en) | 2012-02-01 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102965688A (en) * | 2012-12-10 | 2013-03-13 | 重庆优萃科技有限公司 | Method for preparing p-benzoquinone by electrocatalytic oxidation of phenylamine |
| CN102976914B (en) * | 2012-12-17 | 2015-01-07 | 重庆优萃科技有限公司 | Method for preparing p-benzoquinone |
| CN105011237A (en) * | 2015-06-30 | 2015-11-04 | 天津春发生物科技集团有限公司 | Natural laminaria japonica paste preparation method |
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2007
- 2007-06-15 CN CN2007100524863A patent/CN101081809B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 朱国华等.苯胺法生产对苯二胺的工艺综述.《化学工业与工程技术》.1996,第17卷(第2期),46－49. * |
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