CN109320111A - A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite - Google Patents
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite Download PDFInfo
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- CN109320111A CN109320111A CN201811286011.5A CN201811286011A CN109320111A CN 109320111 A CN109320111 A CN 109320111A CN 201811286011 A CN201811286011 A CN 201811286011A CN 109320111 A CN109320111 A CN 109320111A
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- ardealite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/005—Preparing or treating the raw materials
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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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- 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
- C01P2006/82—Compositional purity water content
Abstract
The invention discloses the methods of titanium pigment and fluorine in a kind of stabilization/solidification ardealite, which comprises the following steps: 1) ardealite is placed in container A, under stirring, after water is added into container A, mixture A is added, mixture B is obtained after stirring；The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；The weight ratio of the ardealite and water is 1 ︰ 2.5~3；The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；The weight ratio of the mixture A and ardealite is (0.5~1) ︰ 100；2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, obtains mixture；The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 5~10 ︰ 1；3) by mixture obtained in step 2) under stirring, discharging is carried out after reacting 2~3h, is obtained by the mixture after stabilization/solidification.
Description
Technical field
The present invention relates to stable/cured processing method field of solid waste, in particular to a kind of stabilization/solidification ardealites
The method of middle titanium pigment and fluorine.
Background technique
Ardealite is a kind of industrial solid castoff of generation during Wet-process Phosphoric Acid Production.They are filled from filtering just
It sets when filtering out, moisture content in mass is up to 25~30% and (therefore " fresh ardealite " is referred to as, to be different from
Dry ardealite without Free water).The waste residue is weakly acidic, and chemical analysis is complicated；Including the titanium pigment that left behind
(P2O5) and in the form of ionic state existing for fluorine.
For at this stage, there are mainly two types of the processing modes of ardealite: stockpiling processing is comprehensively utilized with recycling.According to system
The ardealite of meter, China's stockpiling processing accounts for about the 90% of its total yield, and only only least a portion of ardealite can be integrated into benefit
With.If ardealite heap is put away, titanium pigment and fluorine etc. will gradually be transferred to soil, the underground on periphery under rain drop erosion
In water and river, and environment will be caused greatly pollute-not only to have caused soil pollution, but also cause water eutrophication — that is, person who happens to be on hand for an errand
Use recovering means, the titanium pigment and fluorine equal size in ardealite are also higher, with the extension of time, titanium pigment and
Fluorine etc. still can be collected in the environment such as underground water and pollute.
On the one hand titanium pigment and the fluorine etc. to avoid remaining gather in the environment such as underground water, are also on the other hand safety
Ground resource utilization ardealite (for example, as one of filler in construction material and roadbed material), then, people are just
It uses again and stabilization/curing process is carried out to it, i.e., convert insoluble substance (practise and claim " fixation ") for soluble pollutants
Measure.
In the prior art include a kind of method of impurity in inerting ardealite, specifically uses alkyl, alkenyl and/or the alkane of ammonia
01 derivatives individually or with being combined with each other carry out individually pre-processing for a long time, or pass through together with standard analysis in process
Injection, mutually blending or mutually grinding ardealite is handled, with formed stable ammonia derivative intermediary phosphate and/or
Villiaumite.The prior art achieves preferable technical effect really, however, the prior art can not but reduce ardealite simultaneously
Moisture content, to ardealite carry out harmless treatment obtain it is thorough not enough, meanwhile, this technique is the complex process of high energy consumption.
In conclusion needing a kind of method of titanium pigment and fluorine in stabilization/solidification ardealite in the prior art.
Summary of the invention
Present invention aim to address problems of the prior art, providing can in a kind of stabilization/solidification ardealite
The method of dissolubility phosphorus and fluorine.
To realize the present invention purpose and the technical solution adopted is that such, it is soluble in a kind of stabilization/solidification ardealite
The method of phosphorus and fluorine, which comprises the following steps:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The weight ratio of the ardealite and water is 1 ︰ 2.5~3；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is (0.5~1) ︰ 100；
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 5~10 ︰ 1；
3) by mixture obtained in step 2) under stirring, react 2~3h after carry out discharging, Gu obtain by stabilization/
Mixture after change.
Further, the ardealite in the step 1) is solid, and the water content of the ardealite is 20%~30%.
Further, in the stirring in the step 1): stirring rate is 100~200r/min.
Further, in the whipping process in the step 2): stirring rate is 100~200r/min；Hydrophobicity table is added
Mixing time after the activating agent of face is 1.5~2h.
It is worth noting that: in practice if encounter ardealite be dissolved in after water it is acid excessively high, in order to guarantee that ardealite mixes
Material is in alkaline environment, and the dosage of calcium hydroxide must also increase.
In the present invention, that play so-called " fixation " to titanium pigment, fluorine in ardealite is CaCO3、MgCO3And Ca
(OH)2, stabilization/curing reaction formula is as follows:
Ca2++PO4 3-+H2O→CaHPO4.2H2O↓
Ca2++PO4 3-+H2O→Ca3(PO4)2.2H2O↓
Mg2++PO4 3-+H2O→Mg3(PO4)2.2H2O↓
Mg2++PO4 3-+H2O→MgHPO4.2H2O↓
Ca (OH) in inorganic agent2There are also the effect that mixture is alkalinity is adjusted, water-soluble fluorine can be made under alkaline environment
Stabilization/solidification, reactional equation are as follows:
Ca2++F-→CaF2↓
Mg2++F-→MgF2↓
And dimethyl silicone polymer is mainly the surface chemistry behavior for regulating and controlling ardealite system for handling, reduces containing for ardealite
Water rate.
The mixture before step 3) is dried by stabilization/curing process, in the hydrated adhesive that will not be re-dissolved in water
Solidifying shape.Wherein contain double salt wagnerite (Mg (PO not soluble in water4)2.2H2O), phosphorite (CaHPO4.2H2O), magnesium monohydrogen phosphate
Hydrate (MgHPO4.2H2O), firefly calcium stone (CaF2) and firefly magnesite (MgF2) etc. compounds and some other impurity.
Effect of the invention is unquestionable, the invention has the following advantages that
1) compared with prior art, the present invention can not only " fixation " titanium pigment, fluorine, while can also reduce ardealite
Moisture content；
2) present invention is very beneficial for carrying out resource utilization to ardealite, for example, as construction material and roadbed
One of filler in material；
3) technical solution of the present invention also has processing technological flow simple, and easy-operating advantage is especially advantageous for industrializing
It promotes.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention only
It is limited to following embodiments.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and used
With means, various replacements and change are made, should all include within the scope of the present invention.
Embodiment 1:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is 0.5 ︰ 100；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 5 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 1；
Table 1
| Embodiment 1 | Comparative example 1 | |
| Titanium pigment content (%) in ardealite | 0.65 | 0.87 |
| Titanium pigment curing degree (%) | 25.29 | / |
| Soluble fluoride content (%) in ardealite | 0.33 | 0.53 |
| Soluble fluoride curing degree (%) | 37.74 | / |
| Ardealite moisture content (%) | 20.1 | 20.7 |
| Ardealite moisture content reduced rate (%) | 2.90 | / |
Embodiment 2:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is 0.5 ︰ 100；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 8 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 2；
Table 2
Embodiment 3:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
Weight ratio (0.5 ︰ 100 of the mixture A and ardealite；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 10 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 3；
Table 3
| Embodiment 3 | Comparative example 1 | |
| Titanium pigment content (%) in ardealite | 0.62 | 0.87 |
| Titanium pigment curing degree (%) | 28.74 | / |
| Soluble fluoride content (%) in ardealite | 0.30 | 0.53 |
| Soluble fluoride curing degree (%) | 43.40 | / |
| Ardealite moisture content (%) | 19.1 | 20.7 |
| Ardealite moisture content reduced rate (%) | 7.73 | / |
Embodiment 4:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is 0.67 ︰ 100；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 5 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 4；
Table 4
| Embodiment 4 | Comparative example 1 | |
| Titanium pigment content (%) in ardealite | 0.52 | 0.87 |
| Titanium pigment curing degree (%) | 40.23 | / |
| Soluble fluoride content (%) in ardealite | 0.26 | 0.53 |
| Soluble fluoride curing degree (%) | 50.94 | / |
| Ardealite moisture content (%) | 18.8 | 20.7 |
| Ardealite moisture content reduced rate (%) | 9.18 | / |
Embodiment 5:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is 0.67 ︰ 100；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 8 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 5；
Table 5
| Embodiment 5 | Comparative example 1 | |
| Titanium pigment content (%) in ardealite | 0.46 | 0.87 |
| Titanium pigment curing degree (%) | 47.13 | / |
| Soluble fluoride content (%) in ardealite | 0.23 | 0.53 |
| Soluble fluoride curing degree (%) | 56.60 | / |
| Ardealite moisture content (%) | 18.5 | 20.7 |
| Ardealite moisture content reduced rate (%) | 10.63 | / |
Embodiment 6:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is 0.67 ︰ 100；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 10 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 6；
Table 6
| Embodiment 6 | Comparative example 1 | |
| Titanium pigment content (%) in ardealite | 0.42 | 0.87 |
| Titanium pigment curing degree (%) | 51.72 | / |
| Soluble fluoride content (%) in ardealite | 0.21 | 0.53 |
| Soluble fluoride curing degree (%) | 60.38 | / |
| Ardealite moisture content (%) | 18.3 | 20.7 |
| Ardealite moisture content reduced rate (%) | 11.59 | / |
Embodiment 7:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is 0.67 ︰ 100；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 5 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 7；
Table 7
| Embodiment 7 | Comparative example 1 | |
| Titanium pigment content (%) in ardealite | 0.39 | 0.87 |
| Titanium pigment curing degree (%) | 55.17 | / |
| Soluble fluoride content (%) in ardealite | 0.14 | 0.53 |
| Soluble fluoride curing degree (%) | 73.58 | / |
| Ardealite moisture content (%) | 18.1 | 20.7 |
| Ardealite moisture content reduced rate (%) | 12.56 | / |
Embodiment 8:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is 1 ︰ 100；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 8 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 8；
Table 8
| Embodiment 8 | Comparative example 1 | |
| Titanium pigment content (%) in ardealite | 0.35 | 0.87 |
| Titanium pigment curing degree (%) | 59.77 | / |
| Soluble fluoride content (%) in ardealite | 0.12 | 0.53 |
| Soluble fluoride curing degree (%) | 77.36 | / |
| Ardealite moisture content (%) | 17.9 | 20.7 |
| Ardealite moisture content reduced rate (%) | 13.53 | / |
Embodiment 9:
A kind of method of titanium pigment and fluorine in stabilization/solidification ardealite, the inorganic agent used includes calcium carbonate
(CaCO3), magnesium carbonate (MgCO3), calcium hydroxide (Ca (OH)2) and dimethyl silicone polymer, which is characterized in that including following step
It is rapid:
1) ardealite is placed in container A, under stirring, after water is added into container A, adds mixture A, stir
Mixture B is obtained after mixing；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The water content of the ardealite is 20%~30%；
The weight ratio of the ardealite and water is 1 ︰ 2.5；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is 1 ︰ 100；
In the stirring: stirring rate 100r/min.
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, is mixed
Material；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 10 ︰ 1；
In the whipping process: stirring rate 100r/min；
Mixing time after hydrophobic surfactant is added is 2h；
3) mixture obtained in step 2) is reacted, discharging is carried out after 2~3h, obtained by mixed after stabilization/solidification
Close material.
The present embodiment first passes through calcium carbonate, magnesium carbonate, soluble in calcium hydroxide mixed processing agent stabilization/solidification ardealite
Then phosphorus, fluorine control ardealite moisture content by surfactant dimethyl silicone polymer.
After step 2), according to the measurement of attached water in GB/T 23456-2009 " ardealite ", five oxidation two of water solubility
Phosphorus (P2O5) and the measuring method of water-soluble fluorine (F) measure the moisture content, solvable of the ardealite before and after stabilization/curing process respectively
Property phosphorus and water-soluble fluorine concentration, calculate the reduced rate of titanium pigment, the curing degree of fluorine and ardealite moisture content.
Verification result is as shown in table 9；
Table 9
As can be seen that passing through calcium carbonate, magnesium carbonate, calcium hydroxide mixture inorganic agent and poly- diformazan from above-mentioned each example
The content of titanium pigment is not more than 0.80% in ardealite after radical siloxane stabilization/curing process, and soluble fluoride content is not yet
Greater than 0.50%, ardealite moisture content is not higher than 25%, titanium pigment in ardealite, fluorine highest curing degree up to 63.22%,
83.02%, minimum also up to 25.29%, 37.74%, the moisture content of ardealite can also be effectively reduced.
I.e. titanium pigment, fluorine and ardealite moisture content comply fully with GB/T in ardealite after stabilization/solidification of the invention
23456-2009 " ardealite " national standard-titanium pigment (0.80%), soluble fluoride (0.50%), moisture content (25%), together
When be conducive to the resource utilization of ardealite.
Claims (4)
1. the method for titanium pigment and fluorine in a kind of stabilization/solidification ardealite, which comprises the following steps:
1) ardealite is placed in container A, under stirring, after water is added into container A, mixture A is added, after stirring
Obtain mixture B；
The mixture A includes by calcium carbonate, magnesium carbonate and calcium hydroxide；
The weight ratio of the ardealite and water is 1 ︰ 2.5~3；
The weight ratio of the calcium carbonate, magnesium carbonate and calcium hydroxide is 1 ︰, 1 ︰ 1；
The weight ratio of the mixture A and ardealite is (0.5~1) ︰ 100；
2) under stirring, hydrophobic surfactant is added into container A, continues stirring until uniformly, obtains mixture；
The hydrophobic surfactant is dimethyl silicone polymer；
The w/v (mg ︰ L) of the mixture B and dimethyl silicone polymer is 5~10 ︰ 1；
3) by mixture obtained in step 2) under stirring, discharging is carried out after reacting 2~3h, is obtained by after stabilization/solidification
Mixture.
2. the method for titanium pigment and fluorine in a kind of stabilization/solidification ardealite according to claim 1, it is characterised in that:
Ardealite in the step 1) is solid, and the water content of the ardealite is 20%~30%.
3. the method for titanium pigment and fluorine in a kind of stabilization/solidification ardealite according to claim 1, it is characterised in that:
In stirring in the step 1): stirring rate is 100~200r/min.
4. the method for titanium pigment and fluorine in a kind of stabilization/solidification ardealite according to claim 1, it is characterised in that:
In whipping process in the step 2): stirring rate is 100~200r/min；Stirring after hydrophobic surfactant is added
Time is 1.5~2h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110467168A (en) * | 2019-09-19 | 2019-11-19 | 中南大学 | The recovery method of titanium pigment in a kind of ardealite |
| CN112479614A (en) * | 2020-12-01 | 2021-03-12 | 济南大学 | Treating agent for soluble phosphorus and fluorine in solidified gypsum and solidification method and application thereof |
| CN112808736A (en) * | 2020-12-21 | 2021-05-18 | 贵州昊华工程技术有限公司 | Purification and harmless treatment method of phosphogypsum |
| CN113371782A (en) * | 2021-06-19 | 2021-09-10 | 昆明理工大学 | Material for filtering leaching solution in phosphogypsum slag yard |
| WO2022036923A1 (en) * | 2020-08-20 | 2022-02-24 | 李思言 | Technological process for changing physical and chemical properties of new phosphogypsum by using calcium hydroxide |
| CN114231175A (en) * | 2021-10-29 | 2022-03-25 | 宜都兴发化工有限公司 | Anti-caking agent for phosphogypsum and preparation method and use method thereof |
| CN116285670A (en) * | 2023-03-28 | 2023-06-23 | 贵州大学 | Preparation method of beta-semi-hydrated phosphogypsum surface hybridization nano silicon dioxide hydrophobic self-cleaning coating |
| CN117383856A (en) * | 2023-09-20 | 2024-01-12 | 贵州七通实业有限公司 | Harmless treatment method and application of barium slag |
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| CN110467168A (en) * | 2019-09-19 | 2019-11-19 | 中南大学 | The recovery method of titanium pigment in a kind of ardealite |
| WO2022036923A1 (en) * | 2020-08-20 | 2022-02-24 | 李思言 | Technological process for changing physical and chemical properties of new phosphogypsum by using calcium hydroxide |
| CN112479614A (en) * | 2020-12-01 | 2021-03-12 | 济南大学 | Treating agent for soluble phosphorus and fluorine in solidified gypsum and solidification method and application thereof |
| CN112808736A (en) * | 2020-12-21 | 2021-05-18 | 贵州昊华工程技术有限公司 | Purification and harmless treatment method of phosphogypsum |
| CN113371782A (en) * | 2021-06-19 | 2021-09-10 | 昆明理工大学 | Material for filtering leaching solution in phosphogypsum slag yard |
| CN113371782B (en) * | 2021-06-19 | 2022-05-31 | 昆明理工大学 | Material for filtering leaching solution in phosphogypsum slag yard |
| CN114231175A (en) * | 2021-10-29 | 2022-03-25 | 宜都兴发化工有限公司 | Anti-caking agent for phosphogypsum and preparation method and use method thereof |
| CN116285670A (en) * | 2023-03-28 | 2023-06-23 | 贵州大学 | Preparation method of beta-semi-hydrated phosphogypsum surface hybridization nano silicon dioxide hydrophobic self-cleaning coating |
| CN116285670B (en) * | 2023-03-28 | 2023-08-29 | 贵州大学 | Preparation method of beta-semi-hydrated phosphogypsum surface hybridization nano silicon dioxide hydrophobic self-cleaning coating |
| CN117383856A (en) * | 2023-09-20 | 2024-01-12 | 贵州七通实业有限公司 | Harmless treatment method and application of barium slag |
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