CN109987593A - A kind of friendly process of phosphorus mud recycling yellow phosphorus - Google Patents
A kind of friendly process of phosphorus mud recycling yellow phosphorus Download PDFInfo
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- CN109987593A CN109987593A CN201910311308.0A CN201910311308A CN109987593A CN 109987593 A CN109987593 A CN 109987593A CN 201910311308 A CN201910311308 A CN 201910311308A CN 109987593 A CN109987593 A CN 109987593A
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- phosphorus
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- yellow phosphorus
- ethyl alcohol
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
- C01B25/027—Preparation of phosphorus of yellow phosphorus
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of friendly process of phosphorus mud recycling yellow phosphorus, include the following steps: that phosphorus mud is put into warm water by S1., flood phosphorus mud completely in water；S2. ethyl alcohol is added and stirs, reaction temperature is controlled at 44.1-78.4 DEG C；S3. after standing, there is layering liquid, take upper, middle and lower layer object respectively；S4. recycling storage is carried out to middle layer thing liquid state yellow phosphorus；S5. hot water injection is carried out to lower layer's object black residue, collects flushing liquor；S6. flushing liquor is extracted with ethyl alcohol, collects liquid phosphor.The rate of recovery of yellow phosphorus is improved by multiple circulation and stress using present invention recycling yellow phosphorus；And recycling yellow phosphorus technique is friendly process, does not postback raw secondary pollution.
Description
Technical field
The present invention relates to yellow phosphorus recovery technology fields, and in particular to a kind of friendly process of phosphorus mud recycling yellow phosphorus.
Background technique
It is white to light yellow crisp waxy solid that yellow phosphorus, which is called white phosphorus, 44.1 DEG C of fusing point, 280 DEG C of boiling point, 1.82 grams of density/
cm3.White phosphorus is very active, it is necessary to be stored in water, people sucks 0.1 gram of white phosphorus and will be poisoned to death.White phosphorus is in not air
Under the conditions of, it is heated to 250 DEG C or red phosphorus will be transformed under light illumination.Red phosphorus is nontoxic, is heated to 400 DEG C or more and just catches fire.?
Under high pressure, white phosphorus can be changed into black phosphorus, it has multi-layered network structure, can be conductive, be most stable of in the allotrope of phosphorus.
The method that phosphorus mud is withdrawn at present can be divided into phosphorus mud and burn acid system, physical method separation and chemical method separation.
It is exactly that phosphorus mud is directly burnt that phosphorus mud, which burns acid system, and the phosphorus pentoxide that yellow phosphorus burning generates goes to hydration absorption tower to absorb
As phosphoric acid.The disadvantages of the method are as follows the phosphoric acid quality of recycling is poor, impurity content is high, and the rate of recovery is low, burns in acid residue
It cannot be about absorbed 25% or so containing phosphorus pentoxide.
There are mainly two types of physical method separation, first is that carrying out extraction and separation using organic solvent, organic solvent is usually two sulphur
Change carbon or benzene；Second is that allow phosphorus mud temperature to be maintained at melting temperature or more using the method for filtering, yellow phosphorus is made to be maintained at liquid,
Then separate phosphorus mud and yellow phosphorus by the method filtered, this method can recycle to obtain phosphorus mud, but since filter cloth is regular
It blocks and causes to be difficult to go on smoothly in production.
Chemical method separation mainly has several: first is that passing through the titanium dioxide in alkaline process processing phosphorus mud using soda ash or ammonium hydroxide
Allow yellow phosphorus nature agglomeration separation after silicon；Second is that using allowing yellow phosphorus to agglomerate out after the oxidizer treatments phosphorus mud such as nitric acid, these types side
The method that formula all uses external additive, causes secondary pollution in varying degrees.
The prior art has that secondary pollution is serious or the rate of recovery is low.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of friendly process of phosphorus mud recycling yellow phosphorus.
The purpose of the present invention is achieved through the following technical solutions: a kind of friendly process of phosphorus mud recycling yellow phosphorus, packet
Include following steps:
S1. phosphorus mud is put into warm water, floods phosphorus mud completely in water；
S2. ethyl alcohol is added and stirs, reaction temperature is controlled at 44.1-78.4 DEG C；
S3. after standing, there is layering liquid, take upper, middle and lower layer object respectively；
S4. recycling storage is carried out to middle layer thing liquid state yellow phosphorus；
S5. hot water injection is carried out to lower layer's object black residue, collects flushing liquor；
S6. flushing liquor is extracted with ethyl alcohol, collects liquid phosphor.
Preferably, in the S1, the temperature of the warm water is no more than 78.4 DEG C.
Preferably, in the S2, ethyl alcohol is added while stirring, after ethyl alcohol is added, continues to stir 20min, and mixed
The temperature for closing liquid is controlled at 65-70 DEG C.
Preferably, in the S3, layering liquid includes upper water and alcohol mixeding liquid, middle layer liquid phosphor, lower black
Residue.
Preferably, in the S3, upper water and alcohol mixeding liquid are taken, carries out the separation of ethyl alcohol and water, water after the recovery
S1, S2 are respectively enterd again with ethyl alcohol.
Preferably, in the S4, S1-S3 step is repeated to the liquid phosphor of recycling, to liquid phosphor carry out into
The purification of one step.
Preferably, in the S5,80-100 DEG C of the hot water temperature.
Preferably, in the S6, extracted many times is carried out to the liquid phosphor of collection, purify liquid phosphor.
Preferably, in the friendly process, technique is completed in sealing and circulating space, and water is recycled with ethyl alcohol.
The beneficial effects of the present invention are:
1. improving the rate of recovery of yellow phosphorus by multiple circulation and stress using present invention recycling yellow phosphorus.
2. present invention recycling yellow phosphorus technique is friendly process, raw secondary pollution is not postbacked.
Specific embodiment
Technical solution of the present invention is detailed further below, but protection scope of the present invention is not limited to following institute
It states.
Embodiment 1
A kind of friendly process of phosphorus mud recycling yellow phosphorus, includes the following steps:
S1. the phosphorus mud that 1kg yellow phosphorus content is 29% is put into 67 DEG C of 10L of warm water, floods phosphorus mud completely in water；It is anti-
Only in air, spontaneous combustion occurs for yellow phosphorus exposure.
S2. 5L ethyl alcohol is added and stirs 30min, whipping temp is controlled at 67 DEG C；
S3. after standing, there is layering liquid, take upper, middle and lower layer object respectively；Upper layer is ethanol, and middle layer is liquid phosphor, lower layer
For black residue,
S4. recycling storage is carried out to middle layer thing liquid state yellow phosphorus；
S5. the hot water injection that 90 DEG C are carried out to lower layer's object black residue, collects flushing liquor；To lower layer's object black residue using no filter
Hot water is carried out again after the filtering of the filter plants such as cloth centrifugal separator or folded spiral shell filter press, disk centrifuge, inorganic membrane separator
It rinses, collects flushing liquor, then flushing liquor and filtered fluid again or extracted many times, collect by modes such as ethyl alcohol
Liquid phosphor, to improve the recovery efficiency of yellow phosphorus.
S6. flushing liquor is extracted with ethyl alcohol, collects liquid phosphor.
Furthermore, it is understood that ethyl alcohol is added while stirring in the S2, after ethyl alcohol is added, continue to stir 20min.
Furthermore, it is understood that taking upper water and alcohol mixeding liquid in the S3, the separation of ethyl alcohol and water is carried out, after recycling
Water and ethyl alcohol respectively enter S1, S2 again, recycle a small amount of yellow phosphorus in ethanol, improve the recovery efficiency of yellow phosphorus.
Furthermore, it is understood that S1-S3 step is repeated to the liquid phosphor of recycling in the S4, to liquid phosphor into
Row further purification.
In the present embodiment, the yellow phosphorus finally recycled is 283g, the rate of recovery 97.59%, purity 99.2%.
Furthermore, it is understood that technique is completed in sealing and circulating space in the friendly process, water and ethyl alcohol circulation benefit
With having saved resource, in turn avoided polluting in technique.
The above is only a preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form should not be regarded as an exclusion of other examples, and can be used for other combinations, modifications, and environments, and can be at this
In the text contemplated scope, modifications can be made through the above teachings or related fields of technology or knowledge.And those skilled in the art institute into
Capable modifications and changes do not depart from the spirit and scope of the present invention, then all should be within the scope of protection of the appended claims of the present invention.
Claims (9)
1. a kind of friendly process of phosphorus mud recycling yellow phosphorus, characterized by the following steps:
S1. phosphorus mud is put into warm water, floods phosphorus mud completely in water；
S2. ethyl alcohol is added and stirs, reaction temperature is controlled at 44.1-95 DEG C；
S3. after standing, there is layering liquid, take upper, middle and lower layer object respectively；
S4. recycling storage is carried out to middle layer thing liquid state yellow phosphorus；
S5. hot water injection is carried out to lower layer's object black residue, collects flushing liquor；
S6. flushing liquor is extracted with ethyl alcohol, collects liquid phosphor.
2. a kind of friendly process of phosphorus mud recycling yellow phosphorus according to claim 1, it is characterised in that: in the S1, institute
The temperature for stating warm water is no more than 78.4 DEG C.
3. a kind of friendly process of phosphorus mud recycling yellow phosphorus according to claim 1, it is characterised in that: in the S2, side
It stirs side and ethyl alcohol is added, after ethyl alcohol is added, continue to stir 20min, and the temperature of mixed liquor is controlled at 65-70 DEG C.
4. a kind of friendly process of phosphorus mud recycling yellow phosphorus according to claim 1, it is characterised in that: in the S3, point
Layer liquid includes upper water and alcohol mixeding liquid, middle layer liquid phosphor, lower black residue.
5. a kind of friendly process of phosphorus mud recycling yellow phosphorus according to claim 4, it is characterised in that: in the S3, take
Upper water and alcohol mixeding liquid, carry out the separation of ethyl alcohol and water, and water after the recovery and ethyl alcohol respectively enter S1, S2 again.
6. a kind of friendly process of phosphorus mud recycling yellow phosphorus according to claim 1, it is characterised in that: right in the S4
S1-S3 step is repeated in the liquid phosphor of recycling, is further purified to liquid phosphor.
7. a kind of friendly process of phosphorus mud recycling yellow phosphorus according to claim 1, it is characterised in that: in the S5, institute
State 80-100 DEG C of hot water temperature.
8. a kind of friendly process of phosphorus mud recycling yellow phosphorus according to claim 1, it is characterised in that: right in the S6
The liquid phosphor of collection carries out extracted many times, purifies liquid phosphor.
9. a kind of friendly process of phosphorus mud recycling yellow phosphorus according to any one of claim 1 to 8, it is characterised in that:
In the friendly process, technique is completed in sealing and circulating space, and water is recycled with ethyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910311308.0A CN109987593A (en) | 2019-04-18 | 2019-04-18 | A kind of friendly process of phosphorus mud recycling yellow phosphorus |
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| CN201910311308.0A CN109987593A (en) | 2019-04-18 | 2019-04-18 | A kind of friendly process of phosphorus mud recycling yellow phosphorus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112408344A (en) * | 2020-09-30 | 2021-02-26 | 无锡中科德芯光电感知技术研究院有限公司 | Method for converting white phosphorus |
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| US3998931A (en) * | 1975-06-30 | 1976-12-21 | American Cyanamid Company | Process for continuous conversion of liquid white phosphorus to red phosphorus in agitated slurry |
| US4258022A (en) * | 1978-09-15 | 1981-03-24 | Hoechst Aktiengesellschaft | Continuous production of phosphine |
| US4299806A (en) * | 1980-12-29 | 1981-11-10 | Stauffer Chemical Company | Decolorization of elemental yellow phosphorus |
| DD236911A1 (en) * | 1985-05-07 | 1986-06-25 | Piesteritz Agrochemie | PROCESS FOR CLEANING YELLOW PHOSPHORUS |
| US4664896A (en) * | 1983-11-14 | 1987-05-12 | Fmc Corporation | Process for purifying yellow phosphorus |
| US5002745A (en) * | 1990-05-07 | 1991-03-26 | Fmc Corporation | Method of separating and recovering phosphorus from phosphorus sludge |
| CN101205056A (en) * | 2007-12-12 | 2008-06-25 | 湖北兴发化工集团股份有限公司 | Method for recovering yellow phosphorus from phosphorus mud with centrifugal separation method |
| CN101289175A (en) * | 2008-06-10 | 2008-10-22 | 昆明理工大学 | Process for removing organics in yellow phosphorus |
| CN103496682A (en) * | 2013-09-16 | 2014-01-08 | 贵州金正大生态工程有限公司 | Method for producing phosphoric acid and jointly producing cement and synthetic ammonia by using phosphorus ores, limestone and silica |
| CN103588185A (en) * | 2013-11-14 | 2014-02-19 | 云南江磷集团股份有限公司 | Method for removing sulfur from yellow phosphorus |
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| CN105293457A (en) * | 2015-11-17 | 2016-02-03 | 雷春生 | Method for preparing high-purity phosphoric pentoxide by utilization of phosphorus mud |
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| US3998931A (en) * | 1975-06-30 | 1976-12-21 | American Cyanamid Company | Process for continuous conversion of liquid white phosphorus to red phosphorus in agitated slurry |
| US4258022A (en) * | 1978-09-15 | 1981-03-24 | Hoechst Aktiengesellschaft | Continuous production of phosphine |
| US4299806A (en) * | 1980-12-29 | 1981-11-10 | Stauffer Chemical Company | Decolorization of elemental yellow phosphorus |
| US4664896A (en) * | 1983-11-14 | 1987-05-12 | Fmc Corporation | Process for purifying yellow phosphorus |
| DD236911A1 (en) * | 1985-05-07 | 1986-06-25 | Piesteritz Agrochemie | PROCESS FOR CLEANING YELLOW PHOSPHORUS |
| US5002745A (en) * | 1990-05-07 | 1991-03-26 | Fmc Corporation | Method of separating and recovering phosphorus from phosphorus sludge |
| CN101205056A (en) * | 2007-12-12 | 2008-06-25 | 湖北兴发化工集团股份有限公司 | Method for recovering yellow phosphorus from phosphorus mud with centrifugal separation method |
| CN101289175A (en) * | 2008-06-10 | 2008-10-22 | 昆明理工大学 | Process for removing organics in yellow phosphorus |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112408344A (en) * | 2020-09-30 | 2021-02-26 | 无锡中科德芯光电感知技术研究院有限公司 | Method for converting white phosphorus |
| 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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Application publication date: 20190709 |