CN105984860A - Method for recovering and refining yellow phosphorus by phosphorus sludge - Google Patents
Method for recovering and refining yellow phosphorus by phosphorus sludge Download PDFInfo
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- CN105984860A CN105984860A CN201510062691.2A CN201510062691A CN105984860A CN 105984860 A CN105984860 A CN 105984860A CN 201510062691 A CN201510062691 A CN 201510062691A CN 105984860 A CN105984860 A CN 105984860A
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Abstract
The invention relates to a method for recovering and refining yellow phosphorus by phosphorus sludge. The method comprises the following steps: heating protective gas, pressuring the protective gas as a phosphorus sludge vaporization heat source, sending the protective gas in a vaporization tower and performing reversed hedge with the phosphorus sludge sent by a phosphorus sludge pump, removing dust in phosphorus steam by a dust-removing device, sending the material in a chilling tower, using water for washing and chilling, preparing a yellow phosphorus product, sending gas in a cooling tower, using water for washing and cooling, recovering the residual yellow phosphorus product, and returning the protective gas to a heater for recycling. According to the characteristic that the phosphorus sludge cannot contact with air, the protective gas is heated and pressured, then is taken as the phosphorus sludge vaporization heat source, the protective gas is recycled, and energy conservation and environment protection are realized; the dust-removing device can thoroughly separate the ash and yellow phosphorus in the phosphorus sludge, the purity of the yellow phosphorus product is increased; the method has the advantages of tight process, continuous and automatic operation, and environmental protection and safety, the production efficiency is greatly increased, the recovery rate of the yellow phosphorus product reaches more than 99%, the pipeline pressure testing and centrifugal fan running realize interconnected control, and the production safety is increased.
Description
Technical field
The invention belongs to the treatment technology of phosphorus ore, a kind of method being specifically related to mud phosphor recovery and refining yellow phosphorus.
Technical background
Mud phosphorus is the waste residue formed during phosphorus production, is made up of element phosphor, dust impurities and water, belongs to dangerous solid waste in phosphorus chemistry industry, produces 1 ton of yellow phosphorus and about produce the mud phosphorus of about 0.3 ton.Processing of mud phosphorus deepens continuously the problem inquired into utilizing always phosphorus production enterprise, and it not only affects the response rate and the production cost of phosphorus during yellow phosphorus industry produces, more likely causes serious environmental pollution.Effectively process and compared with this phosphorus-containing waste slag of good utilisation, be possible not only to better profit from limited phosphate rock resource, improve the response rate of phosphorus, reduce production cost, and its pollution to environment can be eliminated.
Reclaiming refined yellow phosphorus from mud phosphorus is effectively to process and the optimum selection of relatively good utilisation mud phosphorus.Physical of the prior art is to utilize U-shaped pot vaporizer or revolution phosphorus-steaming pot, mud phosphorus heating evaporation is become phosphorous steam, then obtains yellow phosphorus product by washing.Use this technology can realize the device of continuous operation few, and vacuum filtration and filter by phosphorus steam self effusion and all there is pipeline and easily block, cause the potential safety hazard of vaporising device blast.CN203065160 discloses a kind of continuous high-efficient environmental protection phosphorous slurry recovery device, fed from U-shaped pot vaporizer front end by screw(-type) feeder, use combustion gas external heat U-shaped pot vaporizer, in U-shaped pot vaporizer, crutcher is set, phosphorus steam escapes from the top of U-shaped pot evaporator back end, and waste residue is discharged from the bottom of U-shaped pot evaporator back end.This device only provides the content that mud phosphorus heating evaporation becomes phosphorous steam, do not only exist mud phosphorus be heated uneven, unload slag charge difficulty and the low problem of environmental safety, and there is no follow-up flow process, solve pipeline the most at all and easily block, cause the potential safety hazard of vaporising device blast.CN1962418 discloses a kind of mud phosphor recovery and refining method, it adds in mud phosphorus and includes ammonium chloride, silicon dioxide, after the dispersant of kieselguhr and magnesium silicate, mud phosphorus is put into revolution phosphorus-steaming pot and burns steaming, the thick phosphorus collected is respectively at phosphorus-melting groove, refinery pit and pan tank rinse with steam for three times, prepare finished phosphorus, the party's chemical method of the prior art owned by France, not only increase consumption of raw and auxiliary materials, production process is formed new garbage, process the most relatively costly, do not process, cause secondary pollution, and the method is intermittent operation, production efficiency is low, extremely difficult realize closed-loop operation, harm workers ' health, environmental safety is low.
Summary of the invention
A kind of method that it is an object of the invention to provide mud phosphor recovery and refining yellow phosphorus; its thermal source that will vaporize as mud phosphorus after protective gas heating, pressurization; the phosphorous steam removing dust device dedusting of vaporization; yellow phosphorus is reclaimed after quenching column cooling, cooling; gas makes temperature be reduced to room temperature through cooling tower again, and the gas after cooling reclaims and uses.The method effectively overcomes the defect that prior art exists, it is proposed that a kind of safe and environment-friendly, cleaning, the new technical scheme of yellow phosphorus continuously and in high efficiente callback mud phosphorus.
The present invention is achieved through the following technical solutions:
A kind of method of mud phosphor recovery and refining yellow phosphorus, mud phosphorus heating evaporation is become phosphorous steam, removing dust equipment dedusting, again with the phosphorous steam of water wash cooling, make yellow phosphorus product, it is with the prominent distinction of prior art: send into centrifugal blower after protective gas is heated to 500～600 DEG C, protective gas is forced into after 0.1～0.15MPa by centrifugal blower sends into the mud phosphorus reversed hedge come in vaporization tower with the pumping of mud phosphorus, after gained phosphorous steam removing dust equipment dedusting, send into quenching column, wash Quench with water to gas phase temperature≤80 DEG C, prepare yellow phosphorus product, gas sends into cooling tower, again wash with water and be cooled to room temperature, receive residue yellow phosphorus product to the greatest extent, protective gas heater return recycles.
Protective gas includes nitrogen, carbon dioxide and noble gas, is optimal with nitrogen or carbon dioxide.
In production practices, the port of export of vaporization tower and cleaner is mounted on pressure transducer, and with centrifugal blower interlocked control, phosphorous gas is when blocking occurs in gas phase pipeline, the pipeline pressure signal raised can be detected and be sent to the master control set of centrifugal blower immediately, after this master control set will differentiate safely according to data, is automatically turned off centrifugal blower, stop vaporization tower and cleaner and easily blocked because of pipeline, and cause the potential safety hazard of blast.
The present invention fully takes into account mud phosphorus creatively can not vaporize thermal source as mud phosphorus with the feature of air contact after protective gas heating, pressurization, and protective gas recycles, energy-conserving and environment-protective；Lime-ash in mud phosphorus can be separated thoroughly by cleaner used with yellow phosphorus, and yellow phosphorus product purity improves；Overall process is airtight, continuous, automation mechanized operation, and environmental safety is high, and production efficiency is greatly improved, and the response rate of yellow phosphorus product up to >=99%, pipeline pressure detection carries out interlocked control with centrifugal blower operation, further increases the safety of production.
With embodiment, the present invention is illustrated below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Accompanying drawing 1 is the production technological process of the present invention.
Detailed description of the invention:
Following embodiment is further intended to describe in detail and explain the present invention rather than limit the present invention by any way.Those of ordinary skill in the art's any simple modifications made for the present invention and replacement, all should fall under the scope of the present invention.
Embodiment 1: a kind of method of mud phosphor recovery and refining yellow phosphorus, centrifugal blower is sent into after nitrogen or carbon dioxide are heated to 500～530 DEG C, protective gas is forced into after 0.1～0.12MPa by centrifugal blower sends into the mud phosphorus reversed hedge come in vaporization tower with the pumping of mud phosphorus, after gained phosphorous steam removing dust equipment dedusting, send into quenching column, wash Quench with water to gas phase temperature≤70 DEG C, prepare yellow phosphorus product, gas sends into cooling tower, again wash with water and be cooled to room temperature, receive residue yellow phosphorus product to the greatest extent, protective gas heater return recycles, the yellow phosphorus response rate in mud phosphorus is 99.15%.
Embodiment 2: a kind of method of mud phosphor recovery and refining yellow phosphorus, centrifugal blower is sent into after nitrogen or carbon dioxide are heated to 530～560 DEG C, protective gas is forced into after 0.12～0.14MPa by centrifugal blower sends into the mud phosphorus reversed hedge come in vaporization tower with the pumping of mud phosphorus, after gained phosphorous steam removing dust equipment dedusting, send into quenching column, wash Quench with water to gas phase temperature≤75 DEG C, prepare yellow phosphorus product, gas sends into cooling tower, again wash with water and be cooled to room temperature, receive residue yellow phosphorus product to the greatest extent, protective gas heater return recycles, the yellow phosphorus response rate in mud phosphorus is 99.3%.
Embodiment 3: a kind of method of mud phosphor recovery and refining yellow phosphorus, centrifugal blower is sent into after nitrogen or carbon dioxide are heated to 560～600 DEG C, protective gas is forced into after 0.14～0.15MPa by centrifugal blower sends into the mud phosphorus reversed hedge come in vaporization tower with the pumping of mud phosphorus, after gained phosphorous steam removing dust equipment dedusting, send into quenching column, wash Quench with water to gas phase temperature≤80 DEG C, prepare yellow phosphorus product, gas sends into cooling tower, again wash with water and be cooled to room temperature, receive residue yellow phosphorus product to the greatest extent, protective gas heater return recycles, the yellow phosphorus response rate in mud phosphorus is 99.4%.
The technology contents of the most detailed description of the present invention is known technology.
Claims (2)
1. the method for a mud phosphor recovery and refining yellow phosphorus, mud phosphorus heating evaporation is become phosphorous steam, removing dust equipment dedusting, again with the phosphorous steam of water wash cooling, make yellow phosphorus product, it is characterized in that: after protective gas is heated to 500～600 DEG C, send into centrifugal blower, protective gas is forced into after 0.1～0.15MPa by centrifugal blower sends into the mud phosphorus reversed hedge come in vaporization tower with the pumping of mud phosphorus, after gained phosphorous steam removing dust equipment dedusting, send into quenching column, wash Quench with water to gas phase temperature≤80 DEG C, prepare yellow phosphorus product, gas sends into cooling tower, again wash with water and be cooled to room temperature, receive residue yellow phosphorus product to the greatest extent, protective gas heater return recycles.
A kind of method of mud phosphor recovery and refining yellow phosphorus, it is characterised in that: protective gas includes nitrogen, carbon dioxide and noble gas, is optimal with nitrogen or carbon dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510062691.2A CN105984860A (en) | 2015-02-06 | 2015-02-06 | Method for recovering and refining yellow phosphorus by phosphorus sludge |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510062691.2A CN105984860A (en) | 2015-02-06 | 2015-02-06 | Method for recovering and refining yellow phosphorus by phosphorus sludge |
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| CN105984860A true CN105984860A (en) | 2016-10-05 |
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| CN201510062691.2A Pending CN105984860A (en) | 2015-02-06 | 2015-02-06 | Method for recovering and refining yellow phosphorus by phosphorus sludge |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601446A (en) * | 2017-10-23 | 2018-01-19 | 湖北兴发化工集团股份有限公司 | The device and method of yellow phosphorus in continuous multi-stage evaporation recovery phosphorus mud |
| CN108840315A (en) * | 2018-08-07 | 2018-11-20 | 李树云 | A kind of processing unit and processing method of the pernicious gas that phosphorous slurry recovery yellow phosphorus generates |
| CN109110738A (en) * | 2018-08-15 | 2019-01-01 | 成都易态科技有限公司 | Yellow phosphorus deep-purifying method and system |
| CN110615415A (en) * | 2019-09-27 | 2019-12-27 | 成都易态科技有限公司 | Sludge phosphorus treatment system and process |
| CN112355039A (en) * | 2020-12-06 | 2021-02-12 | 贵州福泉川东化工有限公司 | Storage and collection integrated double recovery device and recovery method for yellow phosphorus waste residues |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3684461A (en) * | 1968-11-13 | 1972-08-15 | Mueller Fritz | Process and apparatus for use in the work-up of waste water containing phosphorus sludge |
| CN202575983U (en) * | 2012-04-09 | 2012-12-05 | 昆明海口泽辰化工厂 | Environmental safe type phosphorus recovery device capable of efficiently recovering phosphorus in phosphorus slurry |
| CN203065160U (en) * | 2012-12-18 | 2013-07-17 | 徐剑宏 | Continuous high-efficient and environment-friendly mud phosphorus recovery device |
| CN203128203U (en) * | 2013-01-16 | 2013-08-14 | 湖北兴发化工集团股份有限公司 | Device for extracting yellow phosphorus via reduced pressure distillation of phosphorus sludge |
-
2015
- 2015-02-06 CN CN201510062691.2A patent/CN105984860A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3684461A (en) * | 1968-11-13 | 1972-08-15 | Mueller Fritz | Process and apparatus for use in the work-up of waste water containing phosphorus sludge |
| CN202575983U (en) * | 2012-04-09 | 2012-12-05 | 昆明海口泽辰化工厂 | Environmental safe type phosphorus recovery device capable of efficiently recovering phosphorus in phosphorus slurry |
| CN203065160U (en) * | 2012-12-18 | 2013-07-17 | 徐剑宏 | Continuous high-efficient and environment-friendly mud phosphorus recovery device |
| CN203128203U (en) * | 2013-01-16 | 2013-08-14 | 湖北兴发化工集团股份有限公司 | Device for extracting yellow phosphorus via reduced pressure distillation of phosphorus sludge |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601446A (en) * | 2017-10-23 | 2018-01-19 | 湖北兴发化工集团股份有限公司 | The device and method of yellow phosphorus in continuous multi-stage evaporation recovery phosphorus mud |
| CN107601446B (en) * | 2017-10-23 | 2020-02-07 | 湖北吉星化工集团有限责任公司 | Device and method for continuously recovering yellow phosphorus in phosphorus mud through multistage evaporation |
| CN108840315A (en) * | 2018-08-07 | 2018-11-20 | 李树云 | A kind of processing unit and processing method of the pernicious gas that phosphorous slurry recovery yellow phosphorus generates |
| CN109110738A (en) * | 2018-08-15 | 2019-01-01 | 成都易态科技有限公司 | Yellow phosphorus deep-purifying method and system |
| CN110615415A (en) * | 2019-09-27 | 2019-12-27 | 成都易态科技有限公司 | Sludge phosphorus treatment system and process |
| CN110615415B (en) * | 2019-09-27 | 2022-09-09 | 成都易态科技有限公司 | Sludge phosphorus treatment system and process |
| CN112355039A (en) * | 2020-12-06 | 2021-02-12 | 贵州福泉川东化工有限公司 | Storage and collection integrated double recovery device and recovery method for yellow phosphorus waste residues |
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