CN103738987B - A kind of from without the method preparing magnesiumcarbonate calcium chromium slag - Google Patents
A kind of from without the method preparing magnesiumcarbonate calcium chromium slag Download PDFInfo
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- CN103738987B CN103738987B CN201310737213.8A CN201310737213A CN103738987B CN 103738987 B CN103738987 B CN 103738987B CN 201310737213 A CN201310737213 A CN 201310737213A CN 103738987 B CN103738987 B CN 103738987B
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- Prior art keywords
- chromium
- filtrate
- magnesiumcarbonate
- slag
- precipitation
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- 239000002893 slag Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 29
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 title claims abstract description 23
- 239000001095 magnesium carbonate Substances 0.000 title claims abstract description 23
- 229910000021 magnesium carbonate Inorganic materials 0.000 title claims abstract description 23
- 235000014380 magnesium carbonate Nutrition 0.000 title claims abstract description 23
- 229960001708 magnesium carbonate Drugs 0.000 title claims abstract description 22
- RQLWXPCFUSHLNV-UHFFFAOYSA-N [Cr].[Ca] Chemical compound [Cr].[Ca] RQLWXPCFUSHLNV-UHFFFAOYSA-N 0.000 title claims abstract description 13
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011651 chromium Substances 0.000 claims abstract description 32
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 30
- 239000000706 filtrate Substances 0.000 claims abstract description 24
- 238000001556 precipitation Methods 0.000 claims abstract description 18
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000009467 reduction Effects 0.000 claims abstract description 7
- CSJKPFQJIDMSGF-UHFFFAOYSA-K aluminum;tribenzoate Chemical compound [Al+3].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 CSJKPFQJIDMSGF-UHFFFAOYSA-K 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 5
- KWIPUXXIFQQMKN-UHFFFAOYSA-N 2-azaniumyl-3-(4-cyanophenyl)propanoate Chemical compound OC(=O)C(N)CC1=CC=C(C#N)C=C1 KWIPUXXIFQQMKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229940090948 ammonium benzoate Drugs 0.000 claims abstract description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- -1 iron ion Chemical class 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 3
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical group [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 abstract description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052749 magnesium Inorganic materials 0.000 abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001784 detoxification Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 231100000614 poison Toxicity 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 150000001844 chromium Chemical class 0.000 description 2
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000009628 steelmaking Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229940069428 antacid Drugs 0.000 description 1
- 239000003159 antacid agent Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of from without the method preparing magnesiumcarbonate calcium chromium slag, the method comprises the steps: (1) will be broken without calcium chromium ground-slag; (2) add flooding chromium slag, vat liquor is for subsequent use; (3) by the hexavalent chrome reduction in vat liquor be trivalent chromium precipitation; (4) chromium slag separation of iron, aluminum precipitation after step (2) process; (5) by the precipitate and separate aluminum solutions of step (4); (6) in aluminum solutions, add ammonium benzoate generate aluminum benzoate; (7) collect the filtrate merging of step (3), (4) and (6), add sodium carbonate and obtain magnesiumcarbonate.The inventive method can by containing chromic chromium slag detoxification, and is converted into by the magnesium elements contained and can utilizes and the higher another kind of magnesiumcarbonate of added value, thus turns harm into good, and turns waste into wealth.
Description
Technical field
The invention belongs to chromium slag for comprehensive and utilize technical field, in particular to a kind of from without the method preparing magnesiumcarbonate calcium chromium slag.
Background technology
Chromic salts is important inorganic salt product, in recent years, China produces the producer of chromic salts under departments of government guides, the technique adopted is through technological transformation, most employing calcium-free roasting technique, although comparatively there is calcium sinter process to decrease chromium slag generation, but its chromium slag produced is still containing the poisonous chromic salts of sexavalence, and main moiety is MgO70 ~ 80%, CaO0.5 ~ 1.0%, Fe
2o
36 ~ 12%, SiO
23 ~ 7%, Al
2o
33 ~ 5%, Cr
2o
30.2 ~ 2%, wherein Cr
6+0.2 ~ 0.5%.Owing to having strong toxicity containing excess water-solubility Cr (VI), therefore chromium slag is one of internationally recognized 47 kinds of refuses the most dangerous, is listed in National Hazard refuse.
At present, the hexavalent chrome reduction of poison high in chromium slag, for the technique of the method for disposal majority employing dry reduction of chromium slag, is the trivalent chromium of low toxicity by chromium salt production producer, then as the additive, steel-making agglutinant etc. of manufacture of cement.But be no matter the additive as manufacture of cement or the agglutinant of steel-making, all need and relevant manufacturers collaborative process, often due to problems such as the transport of chromium slag, adding technology, expenses in treating processes, cause cooperation producer not positive, chromium slag after reduction can not obtain disposal enough in time, thus cause the chromium slag muck storage of chromium salt production producer day by day to increase, the pressure grown with each passing day is caused to environment.
Magnesiumcarbonate can be used for medicine intermediate, antacid, siccative, colour protecting agent, carrier, the fast agent of resistive connection; Additive, magnesium elements compensator is made in food; For the production of magnesium chemical reagent in fine chemistry industry; Strengthening agent, weighting agent is made in rubber; Thermal insulation, resistant to elevated temperatures fire-retardant heat-insulation material can be made; As important chemical feedstocks in electric wire manufacturing processed, play surface-brightening effect at enamel pottery; And can be used to manufacture high glass goods, make or manufacture magnesium salts, pigment, paint, daily cosmetics, shipbuilding, boiler, and athlete's wiping hand is used.Therefore, by chromium residue detoxifying process process, a large amount of magnesium contained by it are converted into the higher magnesiumcarbonate of added value, not only solve environmental issue, and be that manufacturer increases economic benefit, comprehensive utilization of resources beyond doubt, energy-saving and cost-reducing good method.
Summary of the invention
In view of without in calcium chromium slag except containing except poisonous sexavalence chromic salts also containing a large amount of elements such as magnesium, iron, aluminium, therefore the object of the invention is to by improving chromium slag detoxification technique, thus provide a kind of from without the method preparing magnesiumcarbonate calcium chromium slag.The method can by containing chromic chromium slag detoxification, and is converted into by the magnesium elements contained and can utilizes and the higher another kind of magnesiumcarbonate of added value, thus turns harm into good, and turns waste into wealth.
In order to realize object of the present invention, contriver is studied by lot of experiments and explores, and finally obtains following technical scheme:
From without the method preparing magnesiumcarbonate calcium chromium slag, comprise the steps:
(1) 250 ~ 320 orders will be broken to without calcium chromium ground-slag;
(2) add flooding chromium slag 2 ~ 3 times, each water consumption is 2 ~ 5 times of the chromium quantity of slag, merges vat liquor, for subsequent use;
(3) vat liquor of step (2) is heated to 60 ~ 70 DEG C, adds sodium sulfide solution, be trivalent chromium precipitation by hexavalent chrome reduction, its reaction formula is: 8CrO
4 2-+ 6S
2-+ 23H
2o=8Cr (OH)
3↓+3S
2o
3 2-+ 22OH
-, cooling, filters out chromium hydroxide precipitation, and filtrate is retained for subsequent use;
(4) the chromium slag after step (2) process, add water after stirring with concentrated hydrochloric acid or vitriol oil acidifying, the pH value of liquid phase is finally made to reach between 1 ~ 3, the filtrate adjust ph of filtering gained acidizing fluid step (3) reaches between 4 ~ 6, make iron ion, aluminum ion produce red precipitate to separate out, filter gained filtrate with between the filtrate adjust ph of step (3) to 9 ~ 10, continue process chromium according to step (3);
(5) red precipitate of step (4) is got, progressively be added under stirring in 10-30% dilute phosphoric acid solution, and constantly adopt dilute phosphoric acid adjustment to make aqueous pH values remain between 1 ~ 3, the red precipitate added progressively dissolves and after being all converted into white precipitate, stop stirring, leave standstill, filter, obtain tertiary iron phosphate wet feed, filtrate is for subsequent use;
(6) in step (5) gained filtrate, add ammonium benzoate solution, generate aluminum benzoate precipitation, its reaction formula is: 3C
5h
5cOONH
4+ Al
3+=Al (C
5h
5cOO)
3↓+3NH
4+, filter, precipitation is dry, obtains aluminum benzoate;
(7) collect step (3), the filtrate of (4) and (6) merges, add sodium carbonate solution and make between the pH value of its solution to 7 ~ 9, produce magnesiumcarbonate precipitation, reaction formula: Mg2++CO32-=MgCO3 ↓, filter, dry magnesiumcarbonate.
Compared with prior art, what the present invention relates to has the following advantages and marked improvement without the technique tool preparing magnesiumcarbonate in calcium chromium slag:
(1) magnesium is generally converted into Mg (OH) by prior art
2, need consumption alkali adjusted to ph, the present invention directly produces magnesiumcarbonate with sodium carbonate, economizes on resources;
(2) magnesiumcarbonate comparatively magnesium hydroxide be easier to produce crystal settling, be convenient to filter, save time and expense;
(3) magnesiumcarbonate has higher marketable value compared with magnesium hydroxide.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is done to describing further, but protection scope of the present invention be not limited to these embodiments.Every do not deviate from the present invention's design change or equivalent substituting include within protection scope of the present invention.
1,100Kg is crushed to 320 orders without calcium chromium slag (being provided by Hubei Zhenhua Chemical Co., Ltd.);
2, first time was with 300Kg water soaking, stirring 2 hours, filtered; Second time 200Kg water soaking, stirring 2 hours, filter, and merges secondary soak solution.
3, upper step alkalescence soak solution is heated to 60 ~ 70 DEG C, add the 30%(mass percent of new preparation) sodium sulfide solution, it is trivalent chromium precipitation by hexavalent chrome reduction, until do not produce precipitation, the consumption of 30% sodium sulfide solution is 4.5Kg, cooling, filters out chromium hydroxide precipitation, and filtrate is retained for subsequent use.
4, the chromium slag after step 2 processes, adds 200Kg water, and the instillation 60Kg vitriol oil, makes the pH value of acidizing fluid reach between 1 ~ 2.Filter, filtrate is separately deposited.Filter residue adds 200Kg water again and stirs, and instills the vitriol oil, keeps solution ph between 1 ~ 2, and maintains 2 hours, and consumption vitriol oil 17Kg, filters.Collect the acidizing fluid that merging two step leaches, regulate potential of hydrogen with step 3 neutral and alkali filtrate, make its pH value reach between 3 ~ 4, make iron ion, aluminum ion produce red precipitate and separate out, filter.Filtrate adds the alkaline filtrate adjust ph of step 3 to 9 ~ 10, continues process chromium according to step 3.
5, the red precipitate of step 4 is got, progressively be added to the 20%(mass percent of stirring) dissolve in phosphoric acid, keep between solution ph to 1 ~ 3, pH value raises then appropriateness and supplements dilute phosphoric acid solution and regulate, add red precipitate all to dissolve, and be converted into white precipitate.After red precipitate all adds, continue to keep between solution ph 1 ~ 3, solution is all colourless, and precipitation all changes white into, and reaction completes, and stops stirring, consumes 20% phosphoric acid solution 67Kg, leave standstill, and completely, filter, obtain tertiary iron phosphate wet feed, filtrate is for subsequent use for precipitation.
6,30%(mass percent is slowly added the filtrate of upper step) ammonium benzoate solution 237Kg, make aluminum ion and its reaction generate aluminum benzoate and precipitate.Filtration drying obtains aluminum benzoate 77.6Kg.
7, collect step 3,4 and 6 filtrate merge, add 40%(mass percent) sodium carbonate solution 400Kg makes between the pH value of its solution to 7 ~ 9, produce magnesiumcarbonate precipitation, filter, in whirlwind tower, be drying to obtain magnesium carbonate powder 137Kg.
Claims (1)
1., from without the method preparing magnesiumcarbonate calcium chromium slag, comprise the steps:
(1) 250 ~ 320 orders will be broken to without calcium chromium ground-slag;
(2) add flooding chromium slag 2 ~ 3 times, each water consumption is 2 ~ 5 times of the chromium quantity of slag, merges vat liquor, for subsequent use;
(3) vat liquor of step (2) being heated to 60 ~ 70 DEG C, adding sodium sulfide solution, is trivalent chromium precipitation by hexavalent chrome reduction, cooling, and filter out precipitation, filtrate is for subsequent use;
(4) the chromium slag after step (2) process, add water after stirring with concentrated hydrochloric acid or vitriol oil acidifying, the pH value of liquid phase is finally made to reach between 1 ~ 3, the filtrate adjust ph of filtering gained acidizing fluid step (3) reaches between 4 ~ 6, make iron ion, aluminum ion produce red precipitate to separate out, filter gained filtrate with between the filtrate adjust ph of step (3) to 9 ~ 10, continue process chromium according to step (3);
(5) red precipitate of step (4) is got, progressively being added to mass percent under stirring is in 10%-30% dilute phosphoric acid solution, and constantly adopt dilute phosphoric acid adjustment to make aqueous pH values remain between 1 ~ 3, the red precipitate added progressively dissolves and after being all converted into white precipitate, leave standstill, filter, obtain tertiary iron phosphate wet feed, filtrate is for subsequent use;
(6) in step (5) gained filtrate, add ammonium benzoate solution, generate precipitation, filter, precipitation is dry, and obtain aluminum benzoate, filtrate is for subsequent use;
(7) collect step (3), the filtrate of (4) and (6) merges, add sodium carbonate solution and make between the pH value of its solution to 7 ~ 9, produce magnesiumcarbonate precipitation, filter, dry magnesiumcarbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310737213.8A CN103738987B (en) | 2013-12-30 | 2013-12-30 | A kind of from without the method preparing magnesiumcarbonate calcium chromium slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310737213.8A CN103738987B (en) | 2013-12-30 | 2013-12-30 | A kind of from without the method preparing magnesiumcarbonate calcium chromium slag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103738987A CN103738987A (en) | 2014-04-23 |
| CN103738987B true CN103738987B (en) | 2016-01-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310737213.8A Expired - Fee Related CN103738987B (en) | 2013-12-30 | 2013-12-30 | A kind of from without the method preparing magnesiumcarbonate calcium chromium slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103738987B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105628A (en) * | 1985-07-06 | 1987-01-14 | 莫玉裔 | The nontoxic processing extraction Ca. and Mg of chromium slag reduction method |
| CN101318188A (en) * | 2008-07-16 | 2008-12-10 | 白向南 | Novel process for innocent treatment and resource regeneration of chromic slag |
| CN102965506A (en) * | 2012-12-14 | 2013-03-13 | 葛新芳 | Method for removing aluminum from rare earth solution by benzoate precipitation method |
-
2013
- 2013-12-30 CN CN201310737213.8A patent/CN103738987B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105628A (en) * | 1985-07-06 | 1987-01-14 | 莫玉裔 | The nontoxic processing extraction Ca. and Mg of chromium slag reduction method |
| CN101318188A (en) * | 2008-07-16 | 2008-12-10 | 白向南 | Novel process for innocent treatment and resource regeneration of chromic slag |
| CN102965506A (en) * | 2012-12-14 | 2013-03-13 | 葛新芳 | Method for removing aluminum from rare earth solution by benzoate precipitation method |
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|---|---|
| CN103738987A (en) | 2014-04-23 |
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