CN111924867A - Process for co-producing polyaluminium chloride by using acid-washed quartz sand - Google Patents
Process for co-producing polyaluminium chloride by using acid-washed quartz sand Download PDFInfo
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- CN111924867A CN111924867A CN202010391600.0A CN202010391600A CN111924867A CN 111924867 A CN111924867 A CN 111924867A CN 202010391600 A CN202010391600 A CN 202010391600A CN 111924867 A CN111924867 A CN 111924867A
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- Prior art keywords
- acid
- quartz sand
- polyaluminium chloride
- washing
- liquid
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 52
- 239000006004 Quartz sand Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 76
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 33
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052742 iron Inorganic materials 0.000 claims abstract description 15
- 239000004576 sand Substances 0.000 claims abstract description 14
- 238000005554 pickling Methods 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 10
- 239000010802 sludge Substances 0.000 claims abstract description 8
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000012452 mother liquor Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 abstract description 42
- 235000006408 oxalic acid Nutrition 0.000 abstract description 14
- 239000002351 wastewater Substances 0.000 abstract description 9
- -1 aluminum ions Chemical class 0.000 abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 239000011575 calcium Substances 0.000 abstract description 3
- YALMXYPQBUJUME-UHFFFAOYSA-L calcium chlorate Chemical compound [Ca+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O YALMXYPQBUJUME-UHFFFAOYSA-L 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000006386 neutralization reaction Methods 0.000 abstract description 2
- 238000011085 pressure filtration Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000292 calcium oxide Substances 0.000 abstract 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract 1
- 239000003814 drug Substances 0.000 abstract 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 4
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 3
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZCLVNIZJEKLGFA-UHFFFAOYSA-H bis(4,5-dioxo-1,3,2-dioxalumolan-2-yl) oxalate Chemical compound [Al+3].[Al+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZCLVNIZJEKLGFA-UHFFFAOYSA-H 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- 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
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a process for coproducing polyaluminium chloride by pickling quartz sand, which comprises pickling, acid adjusting liquid, adding bauxite and calcium chlorate to react to generate liquid polyaluminium chloride, performing pressure filtration to separate sludge, and drying liquid polyaluminium chloride to obtain solid polyaluminium chloride. The invention uses hydrochloric acid to wash sand to replace oxalic acid in the prior art, the price of the hydrochloric acid is far lower than that of the oxalic acid, and calcium oxide is not needed to neutralize the wastewater, so the cost of the medicament is reduced by about 75-90%; meanwhile, a waste water neutralization process is omitted, so that a large amount of equipment investment is reduced, and the equipment cost is greatly reduced; because the acidity of the hydrochloric acid is far stronger than that of the oxalic acid, the contents of impurities such as calcium, aluminum and the like in the quartz sand can be effectively removed, and the quality of the quartz sand is greatly improved; because the waste acid contains a certain amount of iron and aluminum ions, the polyaluminium chloride can be comprehensively utilized and produced, and a part of the cost for purchasing hydrochloric acid is saved.
Description
Technical Field
The invention relates to the technical field of quartz sand purification, in particular to a process for co-producing polyaluminium chloride by using acid-washed quartz sand.
Background
At present, the main technology for purifying the quartz sand is to soak the quartz sand in oxalic acid solution or hydrofluoric acid, utilize the chemical reaction of acid and iron in the quartz sand, and then carry out acid washing, rinsing and other processes to acid-wash the high-iron sand (containing iron 300-.
The defects are that the use of oxalic acid washing sand causes serious increase of production cost because the oxalic acid price is high (the consumption of oxalic acid per ton of quartz sand is about 8-12kg calculated according to the iron content of the quartz sand), and the acid content of the acid washing wastewater is high, and lime is needed to be neutralized and filter-pressed; the prices of oxalic acid and hydrofluoric acid are high, and the cost of the oxalic acid and the hydrofluoric acid is about 45-60 yuan/ton in the quartz sand pickling process, so that the cost of the quartz sand pickling is greatly increased; a large amount of waste water is generated after the oxalic acid and the hydrofluoric acid are acid-washed and needs to be treated, the existing treatment process is to neutralize the waste water by lime water to enable iron ions, oxalate ions and fluoride ions in the waste water to form precipitates, and then the aim of recycling the waste water is achieved through flocculation and pressure filtration, the treatment process consumes a large amount of lime, causes great waste water treatment cost, and generates a large amount of solid waste which cannot be treated; if the quartz sand is pickled by hydrofluoric acid, the inevitable volatilization of the hydrofluoric acid and the residual fluorine ions in the wastewater can cause great and irreversible harm to the health of workers and the environment; if oxalic acid is used, in the pickling process, workers operating on site inevitably inhale a small amount of oxalic acid, and the risk of calculus in each organ of the workers is increased rapidly due to the combination of calcium in vivo; in the process of treating the quartz sand with high aluminum content, aluminum oxalate and aluminum fluoride are formed after acid washing, and particularly, the aluminum fluoride is a precipitate insoluble in acid and alkali, so that equipment and pipelines are easily blocked and damaged, and the aluminum fluoride cannot be rinsed out during rinsing of the quartz sand, thereby seriously affecting the quality of the quartz sand.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a process for co-producing polyaluminium chloride by using acid-washed quartz sand.
The technical scheme adopted by the invention for solving the technical problems is as follows: a process for co-producing polyaluminium chloride by pickling quartz sand comprises the following steps of pickling, acid liquor adjustment, bauxite addition and calcium chlorate reaction to generate liquid polyaluminium chloride, filter pressing to separate sludge, liquid polyaluminium chloride and drying to obtain solid polyaluminium chloride, wherein the specific steps are as follows:
step 1, pickling quartz sand
Adding the crushed quartz sand into an acid washing tank, carrying out acid washing by using hydrochloric acid with the concentration of 20%, and separating the quartz sand and acid mother liquor after acid washing;
step 2 acid washing
Adding water into an acid tank, connecting the acid tank with a circulating water pool, circularly washing the acid tank and quartz sand in the tank with acid, and discharging washing acid water to obtain acid liquid I mixed with acid mother liquor;
step 3, adjusting acid liquor
Adding concentrated hydrochloric acid into the acid solution I to mix into acid solution II with the concentration of 15%, and adding the acid solution II into the reactor;
step 4, producing liquid polyaluminium chloride by reaction
Adding the acid liquor II into a reactor, adding bauxite and calcium aluminate into the reactor, and reacting to generate liquid polyaluminium chloride I;
step 5, filter pressing
And (3) introducing the liquid polyaluminium chloride into a filter press, separating sludge and liquid polyaluminium chloride II, selling the sludge, discharging the liquid polyaluminium chloride II into a storage pool, selling the liquid polyaluminium chloride II, or adding the liquid polyaluminium chloride II into a dryer, drying the solid polyaluminium chloride, and warehousing the qualified solid polyaluminium chloride and selling the solid polyaluminium chloride.
Specifically, in the acid washing process in the step 1, the sand washing tank is heated to 50-60 ℃ and is subjected to acid washing circularly, and the iron content of the quartz sand is tested by using water to wash away acid liquor every 2 hours until the iron content of the quartz sand is reduced to 60-100 ppm.
Specifically, the acid washing process in the step 2 is carried out until the pH value of the acid washing water is 6-7.
Specifically, the content of aluminum oxide in the liquid polyaluminum chloride I is 10%, and the basicity is 30-95%.
Specifically, the concentration of the concentrated hydrochloric acid added in the step 3 is 30-33% of hydrochloric acid.
The invention has the following beneficial effects: the invention uses hydrochloric acid to wash sand to replace oxalic acid in the prior art, the price of the hydrochloric acid (the market price is about 100-; meanwhile, a waste water neutralization process is omitted, so that a large amount of equipment investment is reduced, and the equipment cost is greatly reduced; because the acidity of the hydrochloric acid is far stronger than that of the oxalic acid, the contents of impurities such as calcium, aluminum and the like in the quartz sand can be effectively removed, and the quality of the quartz sand is greatly improved; because the waste acid contains a certain amount of iron and aluminum ions, the polyaluminium chloride can be comprehensively utilized and produced, and a part of the cost for purchasing hydrochloric acid is saved.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to the accompanying drawings.
A process for co-producing polyaluminium chloride by pickling quartz sand comprises the following steps of pickling, acid liquor adjustment, bauxite addition and calcium chlorate reaction to generate liquid polyaluminium chloride, filter pressing to separate sludge, liquid polyaluminium chloride and drying to obtain solid polyaluminium chloride, wherein the specific steps are as follows:
step 1, pickling quartz sand
Adding crushed raw sand (containing 300-800ppm of iron) into a sand washing tank through a sand pump or a belt conveyer, adding the crushed raw sand into an acid washing tank, preparing 20% hydrochloric acid solution from purchased hydrochloric acid (with the content of 30-33%) into the sand washing tank, heating to 50-60 ℃, circularly carrying out acid washing, sampling for 2 hours, washing with water to remove the acid solution to assay the iron content until the iron content is reduced to 60-100ppm of quartz sand, obtaining acid-washed low-iron quartz sand and acid mother liquor, and then pumping the acid mother liquor from an acid discharge port at the lower part of the sand washing tank by using a vacuum pump;
step 2 acid washing
Adding water into an acid tank, preferably quartz sand which is not washed by acid, connecting the acid tank with a circulating water tank through a circulating pump, pumping cleaning acid water into the circulating water tank, adding clear water into the sand washing tank while pumping, recycling, performing circulating acid washing on the acid tank and the quartz sand in the tank, using the sand washing water, cleaning until the pH value of the cleaning acid water is 6-7, and discharging the cleaning acid water as acid liquid I mixed with acid mother liquor;
step 3, adjusting acid liquor
Adding hydrochloric acid with the concentration of 30-33% into the acid liquid I to mix into acid liquid II with the concentration of 15% for later use;
step 4, producing liquid polyaluminium chloride by reaction
Adding the acid liquor II into a reactor, quantitatively adding bauxite and calcium aluminate into the reactor while stirring, reacting until the content of aluminum oxide is 10% and the basicity is 30-95% (detected according to GB/T22627-2014), and discharging to obtain liquid polyaluminium chloride I;
step 5, filter pressing
And (2) introducing the liquid polyaluminium chloride into a filter press, separating sludge and liquid polyaluminium chloride II, selling the sludge, discharging the liquid polyaluminium chloride II into a storage pool, selling the liquid polyaluminium chloride II, or adding the liquid polyaluminium chloride II into a dryer, drying to obtain solid polyaluminium chloride, putting the qualified solid polyaluminium chloride into a warehouse, and selling the solid polyaluminium chloride.
The present invention is not limited to the above embodiments, and any structural changes made under the teaching of the present invention shall fall within the protection scope of the present invention, which is similar or similar to the technical solutions of the present invention.
The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (6)
1. A process for co-producing polyaluminium chloride by using acid-washed quartz sand is characterized in that: the method comprises the following steps:
step 1, pickling quartz sand
Adding the crushed quartz sand into an acid washing tank, carrying out acid washing by using hydrochloric acid with the concentration of 20%, and separating the quartz sand and acid mother liquor after acid washing;
step 2 acid washing
Adding water into an acid tank, connecting the acid tank with a circulating water pool, circularly washing the acid tank and quartz sand in the tank with acid, and discharging washing acid water to obtain acid liquid I mixed with acid mother liquor;
step 3, adjusting acid liquor
Adding concentrated hydrochloric acid into the acid solution I to mix into acid solution II with the concentration of 15%, and adding the acid solution II into the reactor;
step 4, producing liquid polyaluminium chloride by reaction
Adding the acid liquor II into a reactor, adding bauxite and calcium aluminate into the reactor, and reacting to generate liquid polyaluminium chloride I;
step 5, filter pressing
And (3) introducing the liquid polyaluminium chloride into a filter press, and separating sludge and liquid polyaluminium chloride II.
2. The process for co-producing polyaluminum chloride from pickled quartz sand as claimed in claim 1, wherein: in the acid washing process in the step 1, the sand washing tank is heated to 50-60 ℃ and is subjected to acid washing circularly, and during the period, the iron content of the quartz sand is tested by using water to wash away acid liquor every 2 hours until the iron content of the quartz sand is reduced to 60-100 ppm.
3. The process for co-producing polyaluminum chloride from pickled quartz sand as claimed in claim 1, wherein: and (3) washing in the acid washing process in the step (2) until the pH value of the acid washing water is 6-7.
4. The process for co-producing polyaluminum chloride from pickled quartz sand as claimed in claim 1, wherein: the content of aluminum oxide in the liquid polyaluminum chloride I is 10%, and the basicity is 30-95%.
5. The process for co-producing polyaluminum chloride from pickled quartz sand as claimed in claim 1, wherein: the concentration of the concentrated hydrochloric acid added in the step 3 is 30-33% of hydrochloric acid.
6. The process for co-producing polyaluminum chloride from pickled quartz sand as claimed in claim 1, wherein: and adding the liquid polyaluminium chloride II into a dryer, and drying to obtain solid polyaluminium chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010391600.0A CN111924867A (en) | 2020-05-11 | 2020-05-11 | Process for co-producing polyaluminium chloride by using acid-washed quartz sand |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010391600.0A CN111924867A (en) | 2020-05-11 | 2020-05-11 | Process for co-producing polyaluminium chloride by using acid-washed quartz sand |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010391600.0A Pending CN111924867A (en) | 2020-05-11 | 2020-05-11 | Process for co-producing polyaluminium chloride by using acid-washed quartz sand |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1274113A (en) * | 1969-09-24 | 1972-05-10 | Tsniitmash | A liquid self-hardening mixture for the production of foundry cores and moulds and method for the production thereof |
| CN101905898A (en) * | 2010-08-03 | 2010-12-08 | 常州友邦净水材料有限公司 | Utilization method for polymeric aluminium reaction residues |
| CN102701251A (en) * | 2012-07-02 | 2012-10-03 | 广西宇泉水务环保工程有限公司 | Preparation process of polyaluminium chloride |
| CN103964445A (en) * | 2014-05-05 | 2014-08-06 | 临沂晟泉矿业有限公司 | Quartz sand pickling comprehensive recycle method |
| CN105152173A (en) * | 2015-08-06 | 2015-12-16 | 安徽东阳矿业科技有限公司 | Quartz sand pickling circulatory purification technology |
| CN109956582A (en) * | 2017-12-25 | 2019-07-02 | 安徽洁之源环保科技有限公司 | Hydrochloric acid acidleach quartz sand sewage treatment process |
-
2020
- 2020-05-11 CN CN202010391600.0A patent/CN111924867A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1274113A (en) * | 1969-09-24 | 1972-05-10 | Tsniitmash | A liquid self-hardening mixture for the production of foundry cores and moulds and method for the production thereof |
| CN101905898A (en) * | 2010-08-03 | 2010-12-08 | 常州友邦净水材料有限公司 | Utilization method for polymeric aluminium reaction residues |
| CN102701251A (en) * | 2012-07-02 | 2012-10-03 | 广西宇泉水务环保工程有限公司 | Preparation process of polyaluminium chloride |
| CN103964445A (en) * | 2014-05-05 | 2014-08-06 | 临沂晟泉矿业有限公司 | Quartz sand pickling comprehensive recycle method |
| CN105152173A (en) * | 2015-08-06 | 2015-12-16 | 安徽东阳矿业科技有限公司 | Quartz sand pickling circulatory purification technology |
| CN109956582A (en) * | 2017-12-25 | 2019-07-02 | 安徽洁之源环保科技有限公司 | Hydrochloric acid acidleach quartz sand sewage treatment process |
Non-Patent Citations (2)
| Title |
|---|
| 武永爱: "酸溶二步法制备聚合氯化铝的试验研究", 《辽宁化工》, no. 09, 20 September 2011 (2011-09-20), pages 913 - 916 * |
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