CN103213958A - Method for recovering simple-substance phosphorus from sludge phosphorus via terminal membrane microfiltration and application for same - Google Patents
Method for recovering simple-substance phosphorus from sludge phosphorus via terminal membrane microfiltration and application for same Download PDFInfo
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Abstract
The invention discloses a method for recovering simple-substance phosphorus from sludge phosphorus via terminal membrane microfiltration, which is remarkably increased in the recovery rate of simple-substance phosphorus compared with the existing method. The method for recovering simple-substance phosphorus from sludge phosphorus via terminal membrane microfiltration disclosed by the invention comprises the following steps of: firstly, mixing a sludge phosphorus raw material with hot water at 60-90 DEG C, so as to melt and settle simple-substance phosphorus in the sludge phosphorus raw material under the heat insulation of the hot water; secondly, only drawing the melted and settled substances in the mixture aforementioned in a terminal membrane microfiltration device, so as to filter the melted and settled substances by a membrane component at a filter temperature of 50-85 DEG C and under a filter pressure of 0.1-0.3 MPa; and finally, conveying the product passing through the membrane component aforementioned to a phosphorus-receiving tank, and settling at the bottom of the phosphorus-receiving tank to obtain simple-substance phosphorus. A production process adopting the method aforementioned for yellow phosphorus comprises the steps of pouring the raw materials of phosphorite, coke, silica and the like in an electric furnace to react, and then performing spray-cooling on a furnace gas and obtaining crude phosphorus, wherein after that, the crude phosphorus is directly used as a raw material, and the operation is performed according to the method aforementioned for recovering simple-substance phosphorus from sludge phosphorus.
Description
Technical field
The present invention relates to a kind of phosphorus production technology that from mud phosphorus, reclaims elemental phosphorous method and use this method.
Background technology
Yellow phosphorus is the Chemicals of a kind of high energy consumption, high material-consumption, high pollution.Present phosphorus production technology is that phosphorus ore, coke and silica raw material are dropped into the electric furnace reaction in proportion, then furnace gas is sprayed cooling and obtains thick phosphorus, and then make with extra care carrying out two-stage in the thick phosphorus importing refinery pit, finally obtains the yellow phosphorus product.Have the hazardous and noxious substances that quantity is big, kind is many in the said process and produce, as waste water, slag, yellow phosphoric tail gas, mud phosphorus etc.From the angle of recycling economy, these materials all are useful byproducts.At present, mainly realize the comprehensive regulation and the utilization of objectionable impurities by following approach: 1, waste water closed circulation after treatment, realize zero release; 2, slag is widely used in and makes building materials, fertilizer and large-scale dam construction etc.; 3, tail gas now mainly is used as fuel, and the technical research of the production steam that burning.Utilize in the work in the improvement to objectionable impurities, elemental phosphorous recovery is difficult point and emphasis in the mud phosphorus, and it has determined the production cost of phosphorus production enterprise, has determined that also can enterprise sustainable development.Mud phosphorus is the important by-products that produces in the phosphorus production process, is a kind of solid waste of danger.Elemental phosphorous recovery is in the phosphorus production-individual very important problem in the mud phosphorus, and it not only influences the rate of recovery and the production cost of phosphorus in the phosphorus production, more seriously causes serious environmental to pollute and safety problem.Therefore, nearly all phosphorus production producer is all in processing and the utilization of inquiring into mud phosphorus, in the hope of reaching good benefits in environment, economic benefit and social benefit.
Mud phosphorus mainly is made up of elemental phosphorous, solid impurity and water, is particle dust, the SiF in the furnace gas
4The SiO that hydrolysis generates
2Deng the spherical particle that adheres to each other with yellow phosphorus, they are emulsoid or false emulsoid.According to present yellow phosphorus examination technology, it is refining that the mud phosphorus part of formation is put refinery pit into thick phosphorus, and another part is then with being subjected to phosphorus groove overflow water to enter the sewage disposal purification system.Phosphorus content in the mud phosphorus all is very high, and the phosphorus content of the mud phosphorus that produces in the refinery pit can reach 90%; And the mud phosphorus phosphorus content that enters sink drainage is lower, is generally 35-60%; Enter its phosphorus content of grains of sand shape mud phosphorus that trench etc. locates 3-35% is also arranged.Therefore, reclaim the phosphorus in the mud phosphorus, both can realize energy-saving and emission-reduction, economize on resources, can reduce of the pollution of mud phosphorus again environment.Reclaim elemental phosphorous method at present and can be divided into two kinds substantially from mud phosphorus: first kind is direct method, wherein is mainly to steam the phosphorus method, is used to reclaim elemental phosphorous product; Second kind is indirect method (conversion method), wherein is mainly relieving haperacidity method, alkaline purification and oxide treatment method etc., products such as by-product phosphoric acid, hypophosphite, phosphite or phosphoric acid salt.Above-mentioned these methods or exist the elemental phosphorous rate of recovery not high, otherwise have the process complexity, to problem such as Pollution abatement is not thorough.
Summary of the invention
The present invention at first will provide a kind of and reclaim elemental phosphorous method by the terminal membrane microfiltration from mud phosphorus, and the elemental phosphorous rate of recovery of this method is significantly increased than existing methods.It less importantly provides a kind of phosphorus production technology of using aforesaid method the present invention, and this technology is compared and had now technology and omitted two-stage refinery pit and whole mud phosphorus ponds, can save great amount of investment, manpower, water and energy consumption.
The terminal membrane microfiltration that passes through of the present invention reclaims elemental phosphorous method from mud phosphorus, the steps include: at first, and the hot water of mud phosphorus raw material with 60-90 ℃ is mixed, and makes elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction terminal membrane microfiltration device in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.
Adopt the phosphorus production technology of aforesaid method to comprise that raw materials such as phosphorus ore, coke and silica are dropped into electric furnace to react, then furnace gas is sprayed the step of cooling off and obtaining thick phosphorus, after this, directly described thick phosphorus is also operated as follows as raw material: at first, the hot water of thick phosphorus with 60-90 ℃ is mixed, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction terminal membrane microfiltration device in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.
Also will provide a kind of below the present invention and reclaim elemental phosphorous method by the cross-flow membrane micro-filtration from mud phosphorus, the elemental phosphorous rate of recovery of this method is significantly increased than existing methods equally.In addition, also will provide a kind of use to pass through the cross-flow membrane micro-filtration reclaims elemental phosphorous method from mud phosphorus phosphorus production technology, this technology is compared and is had now technology and omitted two-stage refinery pit and whole mud phosphorus ponds, can save great amount of investment, manpower, water and energy consumption.
The cross-flow membrane micro-filtration that passes through of the present invention reclaims elemental phosphorous method from mud phosphorus, the steps include: at first, and the hot water of mud phosphorus raw material with 60-90 ℃ is mixed, and makes elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction cross-flow membrane micro-filtration in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous; Wherein, when filtering with described mixture along the flow rate control on membrane element surface at 0.01-0.5m/s.
Adopt the phosphorus production technology of aforesaid method to comprise that raw materials such as phosphorus ore, coke and silica are dropped into electric furnace to react, then furnace gas is sprayed the step of cooling off and obtaining thick phosphorus, after this, directly described thick phosphorus is also operated as follows as raw material: at first, the hot water of thick phosphorus with 60-90 ℃ is mixed, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction terminal membrane microfiltration device in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.
Above-mentioned term " terminal membrane microfiltration device " obviously is meant and adopts end-filtration mode, filtering accuracy to belong to the interior membrane filter appts of micro-filtration scope.Above-mentioned term " cross-flow membrane micro-filtration " obviously is meant and adopts cross flow filter mode, filtering accuracy to belong to the interior membrane filter appts of micro-filtration scope.Wherein, end-filtration and cross flow filter are the ordinary skill in the art, and its difference is, liquid vertical film element surface motion during end-filtration, and liquid is along the membrane element apparent motion, so cross flow filter more can slow down the formation of cake layer during cross flow filter.In addition, " micro-filtration " typically refers to the filtration of filtering accuracy at the 0.1-20 mu m range." filtering accuracy " is meant among the present invention, and membrane element more than 98%, then is called this particle diameter the filtering accuracy of membrane element to a certain particle diameter particulate clearance.
Actual verification shows, adopts the above-mentioned elemental phosphorous method that reclaims from mud phosphorus, and the elemental phosphorous rate of recovery can reach more than 95%, and additive method only reaches 70% to the elemental phosphorous rate of recovery is the highest at present.New phosphorus production flow process is brief, and working cost is low, the phosphorous recovery height, and the residue phosphorus content is low, and the last handling process of residue is simple and convenient, and safe operation process is reliable, and decontamination comparatively up hill and dale is relatively advanced at present phosphorus production technology.
The present invention is described further below in conjunction with embodiment.Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Embodiment
The present invention reclaims elemental phosphorous method by the terminal membrane microfiltration from mud phosphorus, the steps include: at first, and the hot water of mud phosphorus raw material with 60-90 ℃ is mixed, and makes elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction terminal membrane microfiltration device in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.With the hot water blended main purpose of mud phosphorus raw material and 60-90 ℃, the one, make elemental phosphorous being heated change molten state into so that follow-up filtration, the 2nd, in elemental phosphorous fusion sedimentation with mud phosphorus in colloid separate with solid particulate.After this, crucial skill only is with the fusion sediment suction terminal membrane microfiltration device in the mixture, and avoid slurries suction terminal membrane microfiltration device with fusion sediment top, could guarantee so follow-up can filtering stability, otherwise very easily stop up membrane element will cause filtering the time.By with the fusion sediment under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature after, the elemental phosphorous rate of recovery can be far above present recovery technology.
Another kind of method of the present invention is to reclaim elemental phosphorously from mud phosphorus by the cross-flow membrane micro-filtration, the steps include: at first, and the hot water of mud phosphorus raw material with 60-90 ℃ is mixed, and makes elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction cross-flow membrane micro-filtration in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous; Wherein, when filtering with described mixture along the flow rate control on membrane element surface at 0.01-0.5m/s.Above-mentionedly from mud phosphorus, reclaims elemental phosphorous method by the cross-flow membrane micro-filtration to reclaim elemental phosphorous method from mud phosphorus substantially the same with passing through the terminal membrane microfiltration, the key distinction is when cross flow filter and described mixture need be controlled at 0.01-0.5m/s along the flow velocity (crossflow velocity) on membrane element surface, this crossflow velocity span of control is low-down in present cross flow filter technology, mainly is to require special the setting for adapting to the elemental phosphorous cross flow filter of molten state.
No matter above-mentionedly from mud phosphorus, reclaims elemental phosphorous method by the terminal membrane microfiltration and still pass through the cross-flow membrane micro-filtration and from mud phosphorus, reclaim elemental phosphorous method, the hot water of mud phosphorus raw material with 60-90 ℃ is mixed carrying out, make wherein elemental phosphorous under hot water thermal insulating during the fusion sedimentation, the preferably subsidiary pH value of taking to regulate mixture is to 7.5-8.5 and/or add the assist measure of flocculation agent in mixture, so that the content (mass percent) of fine particle is reduced to below 0.01% in the described fusion sediment; Wherein, described fine particle is meant colloid in the mixture and the particle diameter solid less than 2 μ m.Find that by actual verification the content of fine particle is controlled at 0.01% when following in the fusion sediment, no matter is terminal membrane microfiltration device or cross-flow membrane micro-filtration, the fading period of its filtration flux obviously descends, and filtration efficiency significantly promotes.In addition, no matter be terminal membrane microfiltration device or cross-flow membrane micro-filtration, membrane element is wherein preferably made by sintering metal porous material or sintered ceramic porous material.Wherein, sintering TiAl porous material, sintered stainless steel porous material, sintered ceramic porous material are preferably and select.The present invention also preferably is controlled to be 0.5-10 μ m with the filtering accuracy of membrane element, is preferably 2-8 μ m, guarantees the elemental phosphorous rate of recovery is reached very high level.
From mud phosphorus, reclaim elemental phosphorous method or from mud phosphorus, reclaim elemental phosphorous method by the terminal membrane microfiltration based on above-mentioned by the cross-flow membrane micro-filtration, because these methods have the rate of recovery height to phosphorus, the residue phosphorus content is low, advantages such as the last handling process of residue is simple and convenient, therefore, the present invention further expects existing phosphorus production system is reformed, and promptly saves present two-stage refinery pit and whole mud phosphorus pond, directly handles thick phosphorus with aforesaid method.Phosphorus production technology after the innovation is specially: phosphorus production technology comprises that phosphorus ore, coke and silica raw material are dropped into electric furnace to react, then furnace gas is sprayed the step of cooling off and obtaining thick phosphorus, after this, directly described thick phosphorus is also operated as follows as raw material: at first, the hot water of thick phosphorus with 60-90 ℃ is mixed, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction terminal membrane microfiltration device in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.Perhaps, phosphorus production technology comprises that raw materials such as phosphorus ore, coke and silica are dropped into electric furnace to react, then furnace gas is sprayed the step of cooling off and obtaining thick phosphorus, after this, directly described thick phosphorus is also operated as follows as raw material: at first, the hot water of thick phosphorus with 60-90 ℃ is mixed, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction cross-flow membrane micro-filtration in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous; Wherein, when filtering with described mixture along the flow rate control on membrane element surface at 0.01-0.5m/s.
Based on front alleged cause, preferably the pH value by above-mentioned fusion sedimentation and adjusting mixture adds flocculation agent to 7.5-8.5 and/or in mixture, and the content (mass percent) of fine particle in the described fusion sediment is reduced to below 0.01%; Wherein, described fine particle is meant colloid in the mixture and the particle diameter solid less than 2 μ m.In addition, described membrane element is preferably made by sintering metal porous material or sintered ceramic porous material.The filtering accuracy of membrane element is preferably 0.5-10 μ m, is preferably 2-8 μ m.Certainly, except that sintering metal porous material or sintered ceramic porous material, some high strength, high corrosion resistance and resistant to elevated temperatures organic porous filter material also are possible selections.
Embodiment 1
From mud phosphorus, reclaim elemental phosphorous method by the terminal membrane microfiltration, at first, (mud phosphorus comes from refinery pit, and elemental phosphorous content is 32% with mud phosphorus raw material, pending mud phosphorus total amount is 200kg) mix with 80 ℃ hot water, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only with the fusion sediment in the said mixture (wherein the content of fine particle is 0.012%) suction terminal membrane microfiltration device, make it under the filter pressure of 0.2Mpa, be subjected to the filtration of membrane element with 70 ℃ filtration temperatures, described membrane element adopts the stainless steel porous material to filter chimney filter, and filtering accuracy is 15 μ m; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.The filter film area is 1m
2, filtration time 1h, yellow phosphorus average flux 61.9kg/m
2.h.After testing, the elemental phosphorous rate of recovery is 96.7%.The quality index of product is qualified substantially.
Embodiment 2
From mud phosphorus, reclaim elemental phosphorous method by the terminal membrane microfiltration, at first, (mud phosphorus comes from refinery pit with mud phosphorus raw material, elemental phosphorous content is 32%, pending mud phosphorus total amount is 200kg) mix with 70 ℃ hot water, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein, simultaneously with the pH value to 8 of mixture; Then, only with the fusion sediment in the said mixture (wherein the content of fine particle is 0.008%) suction terminal membrane microfiltration device, make it under the filter pressure of 0.3Mpa, be subjected to the filtration of membrane element with 60 ℃ filtration temperatures, described membrane element adopts the alumina-ceramic porous material to filter chimney filter, and filtering accuracy is 2 μ m; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.The filter film area is 1m
2, filtration time 30min, yellow phosphorus average flux 123.4kg/m
2.h.After testing, the elemental phosphorous rate of recovery is 96.4%.Quality product is up to standard qualified.
Embodiment 3
From mud phosphorus, reclaim elemental phosphorous method by the terminal membrane microfiltration, at first, (mud phosphorus comes from refinery pit with mud phosphorus raw material, elemental phosphorous content is 32%, pending mud phosphorus total amount is 200kg) mix with 65 ℃ hot water, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein, in mixture, add the inorganic flocculating agent PFAS simultaneously; Then, only with the fusion sediment in the said mixture (wherein the content of fine particle is 0.009%) suction terminal membrane microfiltration device, make it under the filter pressure of 0.2Mpa, be subjected to the filtration of membrane element with 55 ℃ filtration temperatures, described membrane element adopts the TiAl porous material to filter chimney filter, and filtering accuracy is 4 μ m; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.The filter film area is 1m
2, filtration time 40min, yellow phosphorus average flux 92.4kg/m
2.h.After testing, the elemental phosphorous rate of recovery is 96.2%.Quality product is up to standard qualified.
Embodiment 4
From mud phosphorus, reclaim elemental phosphorous method by the cross-flow membrane micro-filtration, at first, (mud phosphorus comes from refinery pit, and elemental phosphorous content is 32% with mud phosphorus raw material, pending mud phosphorus total amount is 200kg) mix with 80 ℃ hot water, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only with the fusion sediment in the said mixture (wherein the content of fine particle is 0.009%) suction terminal membrane microfiltration device, make it under the filter pressure of 0.2Mpa, be subjected to the filtration of membrane element with 70 ℃ filtration temperatures, described membrane element adopts the TiAl porous material to filter chimney filter, filtering accuracy is 6 μ m, when filtering with described mixture along the flow rate control on membrane element surface at 0.05m/s; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.The filter film area is 0.5m
2, filtration time 1h, yellow phosphorus average flux 121.9kg/m
2.h.After testing, the elemental phosphorous rate of recovery is 95.2%%.Quality product is up to standard qualified.
Embodiment 5
From mud phosphorus, reclaim elemental phosphorous method by the cross-flow membrane micro-filtration, at first, (mud phosphorus comes from refinery pit with mud phosphorus raw material, elemental phosphorous content is 32%, pending mud phosphorus total amount is 200kg) mix with 60 ℃ hot water, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein, simultaneously with the pH value to 8 of mixture; Then, only with the fusion sediment in the said mixture (wherein the content of fine particle is 0.009%) suction membrane microfiltration device, make it under the filter pressure of 0.3Mpa, be subjected to the filtration of membrane element with 50 ℃ filtration temperatures, described membrane element adopts the TiAl porous material to filter chimney filter, filtering accuracy is 6 μ m, when filtering with described mixture along the flow rate control on membrane element surface at 0.3m/s; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.The filter film area is 0.5m
2, filtration time 1h, yellow phosphorus average flux 122.8kg/m
2.h.After testing, the elemental phosphorous rate of recovery is 95.9%.Quality product is up to standard qualified.
Embodiment 6
Phosphorus production innovation technology: directly with the thick phosphorus in the former phosphorus production technology as filtering raw material and operating as follows: with thick phosphorus (elemental phosphorous content be 91%(all the other be solid impurity and a small amount of water entrainment), thick phosphorus total amount is 100kg) mix with 80 ℃ hot water, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein, simultaneously with the pH value to 8 of mixture; Then, only with the fusion sediment in the said mixture (wherein the content of fine particle is 0.007%) suction terminal membrane microfiltration device, make it under the filter pressure of 0.1Mpa, be subjected to the filtration of membrane element with 70 ℃ filtration temperatures, described membrane element adopts the stainless steel porous material to filter chimney filter, and filtering accuracy is 10 μ m; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.The filter film area is 1m
2, filtration time 20min, yellow phosphorus average flux 268.6kg/m
2.h.After testing, the elemental phosphorous rate of recovery is 98.4%, and the part quality index of product is defective.
Embodiment 7
Phosphorus production innovation technology: directly will show thick phosphorus in the phosphorus production technology: with thick phosphorus (elemental phosphorous content be 91%(all the other be solid impurity and a small amount of water entrainment) as filtering raw material and operating as follows, pending thick phosphorus total amount is 100kg) mix with 70 ℃ hot water, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein, simultaneously with the pH value to 8 of mixture; Then, only with the fusion sediment in the said mixture (wherein the content of fine particle is 0.007%) suction cross-flow membrane micro-filtration, make it under the filter pressure of 0.2Mpa, be subjected to the filtration of membrane element with 60 ℃ filtration temperatures, described membrane element adopts the TiAl porous material to filter chimney filter, filtering accuracy is 6 μ m, when filtering with described mixture along the flow rate control on membrane element surface at 0.05m/s; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.The filter film area is 0.5m
2, filtration time 40min, yellow phosphorus average flux 269.5kg/m
2.h, call parameter such as efficient.After testing, the elemental phosphorous rate of recovery is 98.7%.Quality product is up to standard qualified.
Claims (10)
1. from mud phosphorus, reclaim elemental phosphorous method by the terminal membrane microfiltration, the steps include: at first, the hot water of mud phosphorus raw material with 60-90 ℃ is mixed, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction terminal membrane microfiltration device in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.
2. the terminal membrane microfiltration that passes through as claimed in claim 1 reclaims elemental phosphorous method from mud phosphorus, it is characterized in that: the pH value by above-mentioned fusion sedimentation and adjusting mixture adds flocculation agent to 7.5-8.5 and/or in mixture, and the content (mass percent) of fine particle in the described fusion sediment is reduced to below 0.01%; Wherein, described fine particle is meant colloid in the mixture and the particle diameter solid less than 2 μ m.
3. the terminal membrane microfiltration that passes through as claimed in claim 1 or 2 reclaims elemental phosphorous method from mud phosphorus, it is characterized in that: described membrane element is made by sintering metal porous material or sintered ceramic porous material.
4. the terminal membrane microfiltration that passes through as claimed in claim 1 or 2 reclaims elemental phosphorous method from mud phosphorus, it is characterized in that: the filtering accuracy of described membrane element is 0.5-10 μ m.
5. the terminal membrane microfiltration that passes through as claimed in claim 4 reclaims elemental phosphorous method from mud phosphorus, it is characterized in that: the filtering accuracy of described membrane element is 2-8 μ m.
6. phosphorus production technology, comprise phosphorus ore, coke and silica raw material are dropped into the electric furnace reaction, then furnace gas is sprayed the step of cooling off and obtaining thick phosphorus, it is characterized in that, directly described thick phosphorus is also operated as follows as raw material: at first, the hot water of thick phosphorus with 60-90 ℃ is mixed, make elemental phosphorous fusion sedimentation under hot water thermal insulating wherein; Then, only, make it under the filter pressure of 0.1-0.3Mpa, be subjected to the filtration of membrane element with 50-85 ℃ filtration temperature the fusion sediment suction terminal membrane microfiltration device in the said mixture; At last, will be sent to by the product of above-mentioned membrane element and be subjected to the phosphorus jar, and be subjected to the sedimentation of phosphorus pot bottom to obtain elemental phosphorous.
7. phosphorus production technology as claimed in claim 6, it is characterized in that: the pH value by above-mentioned fusion sedimentation and adjusting mixture adds flocculation agent to 7.5-8.5 and/or in mixture, and the content (mass percent) of fine particle in the described fusion sediment is reduced to below 0.01%; Wherein, described fine particle is meant colloid in the mixture and the particle diameter solid less than 2 μ m.
8. as phosphorus production technology as described in claim 6 or 7, it is characterized in that: described membrane element is made by sintering metal porous material or sintered ceramic porous material.
9. as phosphorus production technology as described in claim 6 or 7, it is characterized in that: the filtering accuracy of described membrane element is 0.5-10 μ m.
10. phosphorus production technology as claimed in claim 9 is characterized in that: the filtering accuracy of described membrane element is 2-8 μ m.
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| CN103964405A (en) * | 2014-04-30 | 2014-08-06 | 成都易态科技有限公司 | Production method for yellow phosphorus |
| CN103964405B (en) * | 2014-04-30 | 2016-11-30 | 成都易态科技有限公司 | A kind of production method of yellow phosphorus |
| CN110615415A (en) * | 2019-09-27 | 2019-12-27 | 成都易态科技有限公司 | Sludge phosphorus treatment system and process |
| CN116143090A (en) * | 2023-04-17 | 2023-05-23 | 陕西燎原净化设备有限公司 | Constant-pressure filtration treatment method and treatment device for phosphorus mud |
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| CN1962418A (en) * | 2006-11-27 | 2007-05-16 | 胡晓丽 | Mud phosphor recovery and refining method |
| CN101343050A (en) * | 2008-09-03 | 2009-01-14 | 湖北三新磷酸有限公司 | Method and equipment for preparing yellow phosphorus or phosphoric acid with vertical enclosed tobacco-partition kiln |
| CN101993155A (en) * | 2009-08-17 | 2011-03-30 | 江西金达莱环保研发中心有限公司 | Method for dephosphorization in sewage |
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| CN103964405A (en) * | 2014-04-30 | 2014-08-06 | 成都易态科技有限公司 | Production method for yellow phosphorus |
| CN103964405B (en) * | 2014-04-30 | 2016-11-30 | 成都易态科技有限公司 | A kind of production method of yellow phosphorus |
| 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 |
| CN116143090A (en) * | 2023-04-17 | 2023-05-23 | 陕西燎原净化设备有限公司 | Constant-pressure filtration treatment method and treatment device for phosphorus mud |
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