CN106744753A - 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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Abstract
The invention discloses a kind of method of phosphorus ore stagewise de-magging, by by the ground phosphate rock that fineness is 80 300 mesh ore pulp is mixed to get with water, ore pulp is squeezed into multi-stag de-magging operation, addition de-magging agent at different levels carry out de-magnesium reaction at a set temperature, control different pH value and the 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 as water of sizing mixing after sedimentation, clarifying treatment by using, or use to complete stagewise de-magging as de-magging agent configuration.The present invention is compared to existing technology, content of magnesium controllable in the concentrate for obtaining, the content of Al, Fe and carbonate is also reduced simultaneously, concentrate after treatment significantly improves foaming phenomena and strainability in wet production, de-magging liquid can be recycled in de-magging operation after treatment, and the method is simple 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, specifically a kind of method of phosphorus ore stagewise de-magging.
Background technology
Phosphate rock resource is limited non-renewable resources, and the phosphate rock resource of China is more in middle and low grade bauxite, and rich ore is few, and is generally
High-magnesium-phosphorus ore, mineral grain is thin, embedding cloth tight, and the impurity content such as Mg is 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 ores of Hunan.During Wet-process Phosphoric Acid Production, major impurity Mg in phosphorus ore,
Fe, Al are brought into phosphoric acid, and these objectionable impurities not only influence the production of phosphoric acid by wet process, and phosphoric acid deep processing economic technology is referred to
Mark also has obvious influence.Current phosphorus ore de-magging method is mainly flotation, reverse flotation, but be difficult by the content of MgO drop to 1% with
Under, and P2O5Loss more than 5%, equipment investment is huge；Existing technique of preparing is mainly flotation, and the method uses extensive, but
Rock phosphate in powder for sedimentary rock type is not applied to simultaneously, and takes up an area the problem that big, water resource waste, flotation agent consumption such as develops at the aspect；
There is highly energy-consuming or technology in other such as high-temperature calcination, photoelectricity selections.
Number of patent application is 201410136999.2 Chinese patent, discloses a kind of side of rock phosphate in powder fluidization de-magging
Method, the method is 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,
It is 35~50 DEG C, reaction time 1.5h, control ph 3~4 to control fluidization reaction temperature；Number of patent application is
201210535053.4 Chinese patent, a kind of method for disclosing 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 de-magging control 40~65 DEG C of temperature, pH be 3~3.5, instead
1~2h between seasonable.
The technical scheme of above-mentioned two patent uses a reactor, and the reaction time is long, and separate unit sets in industrialized production
Standby big, investment is big, is unfavorable for middle control, and solution causes the back-mixing of phosphorus ore, crosses and react and owe reaction.The reaction excessively refers to big
The wherein local sour overrich of reaction causes phosphorus ore main component fluorophosphate to participate in reaction causes phosphorus to lose influence concentrate grade, institute
Stating deficient reaction, to refer to that local acid amount is very few cause the magnesium can not effectively to remove.
The content 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 treatment, especially for high content Mg phosphorus ores effect substantially, enterprise demand can be obtained
Different qualities concentrate.
A kind of method of phosphorus ore stagewise de-magging, comprises the following steps：
(1) size mixing
The ground phosphate rock that fineness is 80~300 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein adding
The volume of the water for entering is 1-2 times of ground phosphate rock weight.
(2) de-magging
Ore pulp is squeezed into multi-stag de-magging operation, addition de-magging at different levels agent carries out de-magnesium reaction at 40-60 DEG C of temperature, controls
Make different pH value and the 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
Used as water of sizing mixing after drop, clarifying treatment, or use is configured as de-magging agent.
Further, the mesh number of ground phosphate rock described in step (1) is 150-250.
Further, in step (2), described multi-stag de-magging operation is to be connected using 2~4 reactive tanks, ore pulp by
Chopped-off head reactive tank enters, and is gone out by final stage reactive tank by middle reactive tanks at different levels, and the ore pulp between reactive tanks at different levels is transmitted as the discrepancy in elevation
Overflow is transmitted with pump.
Further, in step (3), described de-magging agent is sulfuric acid or phosphoric acid, and concentration is 5%~30%, or for each
From sulfuric acid and the nitration mixture of phosphoric acid that concentration is 5%~30%.
Further, in step (2), described temperature is 45-55 DEG C.
Further, the operation for controlling different pH value described in step (2) is：Each order of reaction is with the raising pH of series
Value increases therewith, and chopped-off head controls pH for 1.8~2.5, and it is 3.0~4.0 that final stage control pH, and the second level controls the pH to be during three class control
2.4~3.0, it is 2.3~2.7 that the second level controls pH when level Four is controlled, and it is 2.7~3.2 that the third level controls pH.
Further, the operation that the differential responses time is controlled in step (2) is：Each order of reaction reacts with the raising of series
Time increases therewith, and chopped-off head controls the reaction time for 5~7min, and final stage controls the reaction time for 15~25min, during 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 is controlled
It is 12~20min.
Further, in step (3)
Compared with the prior art, the present invention has advantages below：
1st, the concentrate that the present invention is obtained, content of magnesium controllable is between 0.1%~0.6% in concentrate, and phosphorus ore grade is relative
Raw ore grade powder improves 0.1%~6.3%.
2nd, de-magging liquid of the invention, by being used as water of sizing mixing after sedimentation, clarifying treatment, or configures as de-magging agent
With, can realize recycling, waste liquid is not produced, it is very friendly to environment.
3rd, the present invention also reduces the content of Al, Fe and carbonate while content of magnesium in reducing phosphorus ore.After treatment
Concentrate significantly improves foaming phenomena and strainability in wet production.
4th, the present invention is simple to operate, and equipment is relative to be easy to get, and industrially easily realizes extensive and continuous production, Ke Yi great
Big reduction working time, improve production efficiency.
Brief description of the drawings
Fig. 1 is the process chart of phosphorus ore stagewise de-magging of the present invention
Specific embodiment
With reference to embodiments and accompanying drawing is further described to technical scheme, but claimed scope simultaneously
It is not limited to described.
Embodiment 1
A kind of method of phosphorus ore stagewise de-magging, comprises the following steps：
(1) size mixing
The ground phosphate rock that fineness is 80 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein add
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 operation, addition de-magging at different levels agent (concentration is 5% sulfuric acid solution) is in temperature 40
De-magnesium reaction is carried out at DEG C, the ore pulp between reactive tanks at different levels is transmitted as discrepancy in elevation 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 controls pH, and chopped-off head reactive tank controls the reaction time for 5~7min, end
It is 15~25min that order reaction groove controls the reaction time.
(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
Used as water of sizing mixing after drop, clarifying treatment, or use is configured as de-magging agent.
Embodiment 2
A kind of method of phosphorus ore stagewise de-magging, comprises the following steps：
(1) size mixing
The ground phosphate rock that fineness is 300 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein add
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 operation, addition de-magging at different levels agent (concentration is 30% sulfuric acid solution) is in temperature 60
De-magnesium reaction is carried out at DEG C, the ore pulp between reactive tanks at different levels is transmitted as discrepancy in elevation 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 controls pH, and chopped-off head reactive tank controls the reaction time for 5~7min, end
It is 15~25min that order reaction groove controls the reaction time.
(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
Used as water of sizing mixing after drop, clarifying treatment, or use is configured as de-magging agent.
Embodiment 3
A kind of method of phosphorus ore stagewise de-magging, comprises the following steps：
(1) size mixing
The ground phosphate rock that fineness is 300 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein add
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 operation, addition de-magging at different levels agent (concentration is 5% phosphoric acid solution) is in temperature 55
De-magnesium reaction is carried out at DEG C, the ore pulp between reactive tanks at different levels is transmitted as discrepancy in elevation 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 controls pH, and it is 2.4~3.0 that second level reactive tank controls pH, and chopped-off head is anti-
Groove is answered to control the reaction time for 5~7min, second level reactive tank controls the reaction time for 10~20min, the control of final stage reactive tank
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
Used as water of sizing mixing after drop, clarifying treatment, or use is configured as de-magging agent.
Embodiment 4
A kind of method of phosphorus ore stagewise de-magging, comprises the following steps：
(1) size mixing
The ground phosphate rock that fineness is 150 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein add
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 operation, addition de-magging at different levels agent (concentration is 30% phosphoric acid solution) is in temperature 45
De-magnesium reaction is carried out at DEG C, the ore pulp between reactive tanks at different levels is transmitted as discrepancy in elevation 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 controls pH, and it is 2.4~3.0 that second level reactive tank controls pH, and chopped-off head is anti-
Groove is answered to control the reaction time for 5~7min, second level reactive tank controls the reaction time for 10~20min, the control of final stage reactive tank
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
Used as water of sizing mixing after drop, clarifying treatment, or use is configured as de-magging agent.
Embodiment 5
A kind of method of phosphorus ore stagewise de-magging, comprises the following steps：
(1) size mixing
The ground phosphate rock that fineness is 250 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein add
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 operation, (concentration is 5% phosphoric acid and concentration is 5% for addition de-magging at different levels agent
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 the discrepancy in elevation
Pump is used in overflow, transmission.It is 1.8~2.5 that chopped-off head reactive tank controls pH, and it is 3.0~4.0 second level that final stage reactive tank controls pH
It is 2.3~2.7 that reactive tank controls pH, and it is 2.7~3.2 that third level reactive tank controls pH, and it is 5 that chopped-off head reactive tank controls the reaction time
~7min, second level reactive tank controls the reaction time for 12~18min, the third level reactive tank control reaction time be 12~
18min, it is 15~25min that final stage reactive tank controls the reaction time.
(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
Used as water of sizing mixing after drop, clarifying treatment, or use is configured as de-magging agent.
Embodiment 6
A kind of method of phosphorus ore stagewise de-magging, comprises the following steps：
(1) size mixing
The ground phosphate rock that fineness is 250 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein add
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 operation, (concentration is 5% phosphoric acid and concentration is 30% for addition de-magging at different levels agent
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 the discrepancy in elevation
Overflow is transmitted with pump.It is 1.8~2.5 that chopped-off head reactive tank controls pH, and it is 3.0~4.0, the second level that final stage reactive tank controls pH
It is 2.3~2.7 that reactive tank controls pH, and it is 2.7~3.2 that third level reactive tank controls pH, and it is 5 that chopped-off head reactive tank controls the reaction time
~7min, second level reactive tank controls the reaction time for 10~15min, the third level reactive tank control reaction time be 12~
20min, it is 15~25min that final stage reactive tank controls the reaction time.
(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
Used as water of sizing mixing after drop, clarifying treatment, or use is configured as de-magging agent.
Embodiment 7
A kind of method of phosphorus ore stagewise de-magging, comprises the following steps：
(1) size mixing
The ground phosphate rock that fineness is 80 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein add
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 operation, (concentration is 30% phosphoric acid and concentration is 5% for addition de-magging at different levels agent
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 the discrepancy in elevation
Overflow is transmitted with pump.It is 1.8~2.5 that chopped-off head reactive tank controls pH, and it is 3.0~4.0, the second level that final stage reactive tank controls pH
It is 2.3~2.7 that reactive tank controls pH, and it is 2.7~3.2 that third level reactive tank controls pH, and it is 5 that chopped-off head reactive tank controls the reaction time
~7min, second level reactive tank controls the reaction time for 10~15min, the third level reactive tank control reaction time be 12~
20min, it is 15~25min that final stage reactive tank controls the reaction time.
(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
Used as water of sizing mixing after drop, clarifying treatment, or use is configured as de-magging agent.
With the phosphorus raw ore (content of MgO is 6.8%-6.9%) of same quality, according to the operating condition of embodiment 1 to embodiment 7
And the embodiment 1 that number of patent application is 201410136999.2 is tested, P, Al, Fe and carbonate in detection de-magging liquid
Content, the content of MgO in concentrate, correlated results is summarized as follows shown in table：
From the point of view of experimental result, the present invention obtain concentrate in content of magnesium controllable between 0.1%~0.6%, phosphorus ore product
The relative raw ore grade powder in position improves more than 6%, and demagging effect is substantially better than the implementation that number of patent application is 201410136999.2
Example；Simultaneously the present invention can also the content for reducing Al, Fe and carbonate obvious to original ore powder, the favourable quality that improve concentrate,
And de-magging method of the invention, P element is lost small during de-magging, does not result in waste.
Embodiment 8
Source：By the step 3 of embodiment 1- embodiments 7) in through sedimentation, clarification produce waste water be collected.
Operating condition：The waste water that will be collected, according to the method described in the present invention, waste water is brought and prepares de-magging liquid or straight
Connect and mix as water (raw material) and ground phosphate rock, operated according to embodiment 1- embodiments 7, continue to collect the waste water for producing, weight
Multiple above-mentioned steps carry out the treatment of the recycling of waste water, and number of repetition is 50-70 times.
Contrast experiment 1：According to the embodiment of 201410136999.2 Chinese patent, prepared by the waste liquid that embodiment is obtained
Into 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：After wastewater reuse 50-60 times, operated according to the condition of embodiment 1- embodiments 7, the essence for obtaining
The concentrate that ore deposit and embodiment 1- embodiments 7 are obtained, on the premise of embodiment operating condition is the same, the demagnesium rate of both concentrate is poor
Value illustrates that de-magging effect is similar -0.05%~+0.1%；And the concentrate of the concentrate demagnesium rate than embodiment 7 of contrast experiment 1
Demagnesium rate is low by 1%, illustrates that the de-magging effect of contrast experiment 1 is poor, and 201410136999.2 waste liquid can not be reused.
Claims (7)
1. a kind of method of phosphorus ore stagewise de-magging, it is characterised in that：Comprise the following steps：
(1) size mixing
The ground phosphate rock that fineness is 80~300 mesh is mixed into acquisition ore pulp with water stirring, and preheats ore pulp to 40 DEG C, wherein add
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 operation, addition de-magging at different levels agent carries out de-magnesium reaction at 40-60 DEG C of temperature, and control is each
The different pH value of order reaction groove and reaction time；
(3) solid-liquor separation and de-magging liquid reuse
Solid-liquor separation is carried out using sedimentation or filter type, solid phase is concentrate, liquid phase is de-magging liquid, de-magging liquid is by sedimentation, clear
Used as water of sizing mixing after clear treatment, or use is configured as de-magging agent.
2. the method for a kind 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. the method for a kind 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 operation stated is to be connected using 2~4 reactive tanks, and ore pulp is entered by chopped-off head reactive tank, by middle each order reaction
Groove is gone out by final stage reactive tank, and the ore pulp between reactive tanks at different levels is transmitted as discrepancy in elevation overflow or is transmitted with pump.
4. the method for a kind 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 is sulfuric acid and phosphoric acid that respective concentration is 5%~30%
Nitration mixture.
5. the method for a kind 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.
6. the method for a kind of phosphorus ore stagewise de-magging according to claim 1, it is characterised in that：Institute in the step (2)
That states control, and the operation of different pH value is：Each order of reaction increases therewith with the raising pH value of series, chopped-off head control pH for 1.8~
2.5, it is 3.0~4.0 that final stage controls pH, and it is 2.4~3.0 that the second level controls pH during three class control, second level control when level Four is controlled
PH processed is 2.3~2.7, and it is 2.7~3.2 that the third level controls pH.
7. the method for a kind of phosphorus ore stagewise de-magging according to claim 1, it is characterised in that：Control in the step (2)
The operation of differential responses time processed is：Each order of reaction increases therewith with the raising reaction time of series, during chopped-off head control reaction
Between be 5~7min, final stage control the reaction time for 15~25min, and the second level reaction time is 10~20min during three class control,
The second level reaction time is 10~15min when level Four is controlled, and the third level reaction time is 12~20min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN109573972A (en) * | 2019-01-23 | 2019-04-05 | 山东鲁北企业集团总公司 | A kind of method of mid low grade phosphate rock production phosphoric acid and low silica cream |
| CN112758903A (en) * | 2021-01-27 | 2021-05-07 | 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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