CN106744753B - A kind of method of phosphorus ore stagewise de-magging - Google Patents
A kind of method of phosphorus ore stagewise de-magging Download PDFInfo
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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
- C01B25/01—Treating phosphate ores or other raw phosphate materials to obtain phosphorus or phosphorus compounds
Abstract
The invention discloses a kind of methods of phosphorus ore stagewise de-magging, by the way that ground phosphate rock and water that fineness is 80-300 mesh are mixed to get ore pulp, ore pulp is squeezed into multi-stag de-magging process, addition de-magging agent at different levels carry out de-magnesium reaction at a set temperature, control the different pH value and reaction time of reactive tanks at different levels, solid-liquor separation is carried out with sedimentation or filter type, solid phase is concentrate, liquid phase is de-magging liquid, de-magging liquid uses after sedimentation, clarifying treatment as water of sizing mixing, or configure and use as de-magging agent, to complete stagewise de-magging.The present invention is compared with prior art, content of magnesium is controllable in obtained concentrate, the content of Al, Fe and carbonate is also reduced simultaneously, treated, and concentrate significantly improves foaming phenomena and strainability in wet production, de-magging liquid can recycle in de-magging process after processing, and this method is easy to operate, equipment is easy to get, it is easy to accomplish industrialized production.
Description
Technical field
The present invention relates to phosphorus ore de-magging technical field, the method for specifically a kind of phosphorus ore stagewise de-magging.
Background technique
Phosphate rock resource is limited non-renewable resources, and the phosphate rock resource in China is more in middle and low grade bauxite, and rich ore is few, and is mostly
High-magnesium-phosphorus ore, mineral grain is thin, embedding cloth is close, and the impurity contents such as Mg are higher.As content of MgO is in the peaceful raw ore in Sichuan
7.14%, content of MgO is 6.65% in the Xi Xi raw ore of Hunan.During Wet-process Phosphoric Acid Production, major impurity Mg in phosphorus ore,
Fe, Al are brought into phosphoric acid, these objectionable impurities not only influence the production of phosphoric acid by wet process, but also refer to phosphoric acid deep processing economic technology
Mark also has apparent influence.Phosphorus ore de-magging method is mainly flotation, reverse flotation at present, but be difficult to drop to the content of MgO 1% with
Under, and P2O5Loss 5% or more, equipment investment is huge；Existing technique of preparing is mainly flotation, which uses extensively, but
Rock phosphate in powder for sedimentary rock type is simultaneously not suitable for, and takes up an area the problem of big, water resource waste, flotation agent consumption is developed etc.；
Other such as high-temperature calcinations, photoelectricity sort the problems such as immature there are highly energy-consuming or technology.
The Chinese patent that number of patent application is 201410136999.2, discloses a kind of side of rock phosphate in powder fluidization de-magging
Method, the method are to squeeze into a fluidization flower de-magging device to carry out fluidization de-magging using sulfuric acid or phosphoric acid after miberal powder is sized mixing,
Controlling fluidization reaction temperature is 35~50 DEG C, reaction time 1.5h, controls pH value 3~4；Number of patent application is
201210535053.4 Chinese patent discloses a kind of method of phosphorus ore de-magging and phosphoric acid byproduct ammonium magnesium, de-magging rank in the method
Section be using in one apparatus using sulfuric acid or phosphoric acid carry out carry out de-magging control 40~65 DEG C of temperature, pH be 3~3.5, instead
1~2h between seasonable.
The technical solution of above-mentioned two patent is all made of a reactor, and the reaction time is long, and separate unit is set in industrialized production
Standby big, investment is big, is unfavorable for intermediate control, and solution leads to the back-mixing of phosphorus ore, crosses and react and owe reaction.The reaction excessively refers to big
The sour overrich for reacting wherein part, which causes phosphorus ore main component fluorophosphate to participate in reaction, leads to phosphorus loss influence concentrate grade, institute
It states and owes reaction and refer to that part acid amount very few causes magnesium that cannot effectively remove.
Summary of the invention
In order to solve above-mentioned problem of the prior art, the present invention uses phosphorus ore stagewise de-magging, by stagewise and control,
The content of Mg in phosphorus ore is significantly reduced after processing, it is obvious especially for high-content Mg phosphorus ore effect, enterprise demand can be obtained
Different qualities concentrate.
A kind of method of phosphorus ore stagewise de-magging, comprising the following steps:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 80~300 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein plus
The volume of the water entered is 1-2 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into multi-stag de-magging process, addition de-magging agent at different levels carry out de-magnesium reaction at 40-60 DEG C of temperature, control
Make the different pH value and reaction time of reactive tanks at different levels.
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid is by heavy
It is used after drop, clarifying treatment as water of sizing mixing, or configures and use as de-magging agent.
Further, the mesh number of ground phosphate rock described in step (1) is 150-250.
Further, in step (2), the multi-stag de-magging process is to be connected using 2~4 reactive tanks, ore pulp by
Chopped-off head reactive tank by intermediate reactive tanks at different levels by final stage reactive tank into being gone out, the ore pulp between reactive tanks at different levels is transmitted as height difference
Overflow is transmitted with pump.
Further, in step (3), the de-magging agent is sulfuric acid or phosphoric acid, and concentration is 5%~30%, or is each
From the nitration mixture of sulfuric acid and phosphoric acid that concentration is 5%~30%.
Further, in step (2), the temperature is 45-55 DEG C.
Further, the operation of the different pH value of control described in step (2) are as follows: each order of reaction with series raising pH
Value increases therewith, and it is 1.8~2.5 that chopped-off head, which controls pH, and it is 3.0~4.0 that final stage, which controls pH, and second level control pH is when three class control
2.4~3.0, second level control pH is 2.3~2.7 when level Four controls, and it is 2.7~3.2 that the third level, which controls pH,.
Further, the operation of differential responses time is controlled in step (2) are as follows: each order of reaction is reacted with the raising of series
Time increases therewith, and it is 5~7min that chopped-off head, which controls the reaction time, and it is 15~25min that final stage, which controls the reaction time, when three class control
The second level reaction time is 10~20min, and the second level reaction time is 10~15min, the third level reaction time when level Four controls
For 12~20min.
Further, in step (3)
Compared with the prior art, the invention has the following advantages that
1, the obtained concentrate of the present invention, content of magnesium is controllable between 0.1%~0.6% in concentrate, and phosphorus ore grade is opposite
Raw ore grade powder improves 0.1%~6.3%.
2, de-magging liquid of the invention uses after sedimentation, clarifying treatment as water of sizing mixing, or configures as de-magging agent
With, it can be realized and recycle, do not generate waste liquid, it is very friendly to environment.
3, the present invention also reduces the content of Al, Fe and carbonate in reducing phosphorus ore while content of magnesium.Treated
Concentrate significantly improves foaming phenomena and strainability in wet production.
4, operation of the present invention is simple, and equipment is opposite to be easy to get, industrially extensive and continuous production easy to accomplish, Ke Yi great
In big reduction working time, improve production efficiency.
Detailed description of the invention
Fig. 1 is the process flow chart of phosphorus ore stagewise de-magging of the present invention
Specific embodiment
With reference to embodiments and attached drawing the technical scheme of the present invention will be further described, but claimed range is simultaneously
It is not limited to described.
Embodiment 1
A kind of method of phosphorus ore stagewise de-magging, comprising the following steps:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 80 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein be added
The volume of water is 1 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into two-stage type de-magging process, it is at different levels that de-magging agent (sulfuric acid solution that concentration is 5%) is added in temperature 40
De-magnesium reaction is carried out at DEG C, the ore pulp between reactive tanks at different levels is transmitted as height difference overflow or is transmitted with pump.Chopped-off head reactive tank control
PH processed is 1.8~2.5, and it is 3.0~4.0 that final stage reactive tank, which controls pH, and the chopped-off head reactive tank control reaction time is 5~7min, end
Order reaction slot controls the reaction time as 15~25min.
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid is by heavy
It is used after drop, clarifying treatment as water of sizing mixing, or configures and use as de-magging agent.
Embodiment 2
A kind of method of phosphorus ore stagewise de-magging, comprising the following steps:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 300 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein be added
The volume of water is 2 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into two-stage type de-magging process, it is at different levels that de-magging agent (sulfuric acid solution that concentration is 30%) is added in temperature 60
De-magnesium reaction is carried out at DEG C, the ore pulp between reactive tanks at different levels is transmitted as height difference overflow or is transmitted with pump.Chopped-off head reactive tank control
PH processed is 1.8~2.5, and it is 3.0~4.0 that final stage reactive tank, which controls pH, and the chopped-off head reactive tank control reaction time is 5~7min, end
Order reaction slot controls the reaction time as 15~25min.
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid is by heavy
It is used after drop, clarifying treatment as water of sizing mixing, or configures and use as de-magging agent.
Embodiment 3
A kind of method of phosphorus ore stagewise de-magging, comprising the following steps:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 300 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein be added
The volume of water is 2 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into three-level formula de-magging process, it is at different levels that de-magging agent (phosphoric acid solution that concentration is 5%) is added in temperature 55
De-magnesium reaction is carried out at DEG C, the ore pulp between reactive tanks at different levels is transmitted as height difference overflow or is transmitted with pump.Chopped-off head reactive tank control
PH processed is 1.8~2.5, and it is 3.0~4.0 that final stage reactive tank, which controls pH, and it is 2.4~3.0 that second level reactive tank, which controls pH, and chopped-off head is anti-
Answering the slot control reaction time is 5~7min, and second level reactive tank controls the reaction time as 10~20min, and final stage reactive tank controls
Reaction time is 15~25min.
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid is by heavy
It is used after drop, clarifying treatment as water of sizing mixing, or configures and use as de-magging agent.
Embodiment 4
A kind of method of phosphorus ore stagewise de-magging, comprising the following steps:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 150 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein be added
The volume of water is 1.5 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into three-level formula de-magging process, it is at different levels that de-magging agent (phosphoric acid solution that concentration is 30%) is added in temperature 45
De-magnesium reaction is carried out at DEG C, the ore pulp between reactive tanks at different levels is transmitted as height difference overflow or is transmitted with pump.Chopped-off head reactive tank control
PH processed is 1.8~2.5, and it is 3.0~4.0 that final stage reactive tank, which controls pH, and it is 2.4~3.0 that second level reactive tank, which controls pH, and chopped-off head is anti-
Answering the slot control reaction time is 5~7min, and second level reactive tank controls the reaction time as 10~20min, and final stage reactive tank controls
Reaction time is 15~25min.
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid is by heavy
It is used after drop, clarifying treatment as water of sizing mixing, or configures and use as de-magging agent.
Embodiment 5
A kind of method of phosphorus ore stagewise de-magging, comprising the following steps:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 250 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein be added
The volume of water is 2 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into three-level formula de-magging process, (phosphoric acid and concentration that concentration is 5% are 5% for addition de-magging agent at different levels
The mixed acid solution that sulfuric acid is mixed into) de-magnesium reaction is carried out under temperature 50 C, the ore pulp between reactive tanks at different levels is transmitted as height difference
Overflow or with pump, transmission.It is 1.8~2.5 that chopped-off head reactive tank, which controls pH, and it is 3.0~4.0 second level that final stage reactive tank, which controls pH,
It is 2.3~2.7 that reactive tank, which controls pH, and it is 2.7~3.2 that third level reactive tank, which controls pH, and the chopped-off head reactive tank control reaction time is 5
~7min, second level reactive tank control the reaction time be 12~18min, third level reactive tank control the reaction time be 12~
18min, final stage reactive tank control the reaction time as 15~25min.
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid is by heavy
It is used after drop, clarifying treatment as water of sizing mixing, or configures and use as de-magging agent.
Embodiment 6
A kind of method of phosphorus ore stagewise de-magging, comprising the following steps:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 250 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein be added
The volume of water is 1 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into level Four formula de-magging process, (phosphoric acid and concentration that concentration is 5% are 30% for addition de-magging agent at different levels
The mixed acid solution that sulfuric acid is mixed into) de-magnesium reaction is carried out at 55 DEG C of temperature, the ore pulp between reactive tanks at different levels is transmitted as height difference
Overflow is transmitted with pump.It is 1.8~2.5 that chopped-off head reactive tank, which controls pH, and it is 3.0~4.0 that final stage reactive tank, which controls pH, the second level
It is 2.3~2.7 that reactive tank, which controls pH, and it is 2.7~3.2 that third level reactive tank, which controls pH, and the chopped-off head reactive tank control reaction time is 5
~7min, second level reactive tank control the reaction time be 10~15min, third level reactive tank control the reaction time be 12~
20min, final stage reactive tank control the reaction time as 15~25min.
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid is by heavy
It is used after drop, clarifying treatment as water of sizing mixing, or configures and use as de-magging agent.
Embodiment 7
A kind of method of phosphorus ore stagewise de-magging, comprising the following steps:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 80 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein be added
The volume of water is 2 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into level Four formula de-magging process, (phosphoric acid and concentration that concentration is 30% are 5% for addition de-magging agent at different levels
The mixed acid solution that sulfuric acid is mixed into) de-magnesium reaction is carried out at 40 DEG C of temperature, the ore pulp between reactive tanks at different levels is transmitted as height difference
Overflow is transmitted with pump.It is 1.8~2.5 that chopped-off head reactive tank, which controls pH, and it is 3.0~4.0 that final stage reactive tank, which controls pH, the second level
It is 2.3~2.7 that reactive tank, which controls pH, and it is 2.7~3.2 that third level reactive tank, which controls pH, and the chopped-off head reactive tank control reaction time is 5
~7min, second level reactive tank control the reaction time be 10~15min, third level reactive tank control the reaction time be 12~
20min, final stage reactive tank control the reaction time as 15~25min.
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid is by heavy
It is used after drop, clarifying treatment as water of sizing mixing, or configures and use as de-magging agent.
With the phosphorus raw ore (content of MgO 6.8%-6.9%) of same quality, according to embodiment 1 to the operating condition of embodiment 7
And the embodiment 1 that number of patent application is 201410136999.2 is tested, and P, Al, Fe and carbonate in de-magging liquid are detected
Content, the content of MgO, correlated results are summarized as follows shown in table in concentrate:
Judging from the experimental results, the present invention controllable between 0.1%~0.6%, the phosphorus ore product that obtain content of magnesium in concentrate
The opposite raw ore grade powder in position improves 6% or more, and demagging effect is substantially better than the implementation that number of patent application is 201410136999.2
Example；The content of the invention that Al, Fe and carbonate can also be substantially reduced to original ore powder simultaneously, the advantageous quality for improving concentrate,
And de-magging method of the invention, P element are lost small during de-magging, not will cause waste.
Embodiment 8
Source: the waste water that generation is settled, clarified in 7 step 3) of embodiment 1- embodiment is collected.
Operating condition: by the waste water of collection, according to the method described in the present invention, waste water is brought and prepares de-magging liquid or straight
It connects as water (raw material) and ground phosphate rock mixing, is operated according to embodiment 1- embodiment 7, continue to collect the waste water generated, weight
Multiple above-mentioned steps carry out the processing of the recycling of waste water, and number of repetition is 50-70 times.
Comparative experiments 1: according to the embodiment of 201410136999.2 Chinese patent, prepared by the waste liquid that embodiment is obtained
At de-magging liquid or directly and with the mixing of grade phosphorus mine powder, de-magging operation is carried out according to embodiment 7.
Comparative result: it after wastewater reuse 50-60 times, is operated according to 7 condition of embodiment 1- embodiment, obtained essence
The concentrate that mine and embodiment 1- embodiment 7 obtain, under the premise of embodiment operating condition is the same, the demagnesium rate of the two concentrate is poor
Value illustrates that magnesium removal effect is similar -0.05%~+0.1%；And the concentrate demagnesium rate of comparative experiments 1 is than the concentrate of embodiment 7
Demagnesium rate low 1% illustrates that the magnesium removal effect of comparative experiments 1 is poor, and 201410136999.2 waste liquid cannot reuse.
Claims (5)
1. a kind of method of phosphorus ore stagewise de-magging, it is characterised in that: the following steps are included:
(1) it sizes mixing
Ground phosphate rock and water that fineness is 80~300 mesh are stirred acquisition ore pulp, and preheat ore pulp to 40 DEG C, wherein be added
The volume of water is 1-2 times of ground phosphate rock weight；
(2) de-magging
Ore pulp is squeezed into multi-stag de-magging process, addition de-magging agent at different levels carry out de-magnesium reaction at 40-60 DEG C of temperature, and control is each
The different pH value and reaction time of order reaction slot；
The operation of the different pH value of control are as follows: each order of reaction increases therewith with the raising pH value of series, and chopped-off head controls pH
It is 1.8~2.5, it is 3.0~4.0 that final stage, which controls pH, and second level control pH is 2.4~3.0 when three class control, the when level Four controls
Two-stage control pH is 2.3~2.7, and it is 2.7~3.2 that the third level, which controls pH,；
The operation of the control differential responses time are as follows: each order of reaction increases therewith with the raising reaction time of series, chopped-off head
The control reaction time is 5~7min, and it is 15~25min that final stage, which controls the reaction time, when three class control the second level reaction time be
10~20min, the second level reaction time is 10~15min when level Four controls, and the third level reaction time is 12~20min；
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, and liquid phase is de-magging liquid, and de-magging liquid, which passes through, to be settled, is clear
It is used after clear processing as water of sizing mixing, or configures and use as de-magging agent.
2. a kind of method of phosphorus ore stagewise de-magging according to claim 1, it is characterised in that: institute in the step (1)
The mesh number for stating ground phosphate rock is 150-250.
3. a kind of method of phosphorus ore stagewise de-magging according to claim 1, it is characterised in that: in the step (2), institute
The multi-stag de-magging process stated is to be connected using 2~4 reactive tanks, and ore pulp is by chopped-off head reactive tank by intermediate each order reaction
Slot is gone out by final stage reactive tank, and the ore pulp between reactive tanks at different levels is transmitted as height difference overflow or is transmitted with pump.
4. a kind of method of phosphorus ore stagewise de-magging according to claim 1, it is characterised in that: in the step (2), institute
The de-magging agent stated is sulfuric acid or phosphoric acid, and concentration is 5%~30%, or the sulfuric acid and phosphoric acid that are 5%~30% for respective concentration
Nitration mixture.
5. a kind of method of phosphorus ore stagewise de-magging according to claim 1, it is characterised in that: in the step (2), institute
The temperature stated is 45-55 DEG C.
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| CN109437982A (en) * | 2018-11-12 | 2019-03-08 | 贵州开磷氟硅化工有限责任公司 | A kind of method that phosphorus ore de-magging waste liquid prepares water-soluble ammonium sulphate phosphate fertiliser containing magnesium feed additives |
| CN109573972B (en) * | 2019-01-23 | 2021-05-28 | 山东鲁北企业集团总公司 | Method for producing phosphoric acid and low-silicon gypsum from medium-low grade phosphorite |
| CN112758903B (en) * | 2021-01-27 | 2023-01-31 | 金正大生态工程集团股份有限公司 | Medium-low grade phosphorite pretreatment method |
| CN114436227A (en) * | 2022-02-17 | 2022-05-06 | 四川省汉源化工总厂 | Circulation thickening water-saving and acid-saving technology for magnesium removal liquid |
| CN115520843A (en) * | 2022-09-30 | 2022-12-27 | 昆明川金诺化工股份有限公司 | Method for improving phosphorus yield of low-magnesium phosphorite produced by chemical magnesium removal of magnesium-containing phosphorite |
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| CN103073034A (en) * | 2013-01-17 | 2013-05-01 | 贵州开磷（集团）有限责任公司 | Method for removing magnesium from ultralow-quality phosphate rock and producing magnesium hydroxide |
| CN103950908A (en) * | 2014-04-04 | 2014-07-30 | 贵阳中化开磷化肥有限公司 | Method for fluidization removal of magnesium from phosphate ore |
| CN104445120A (en) * | 2014-11-04 | 2015-03-25 | 湖北祥云(集团)化工股份有限公司 | Co-production method and system of ammonium phosphate and magnesium hydrate |
| CN104876198A (en) * | 2015-05-12 | 2015-09-02 | 贵州开磷集团股份有限公司 | Sodium fluosilicate production-phosphorite demagging combined treatment method |
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