CN1081091C - Process for preparing iron ore antifloating inhibitor - Google Patents
Process for preparing iron ore antifloating inhibitor Download PDFInfo
- Publication number
- CN1081091C CN1081091C CN99103401A CN99103401A CN1081091C CN 1081091 C CN1081091 C CN 1081091C CN 99103401 A CN99103401 A CN 99103401A CN 99103401 A CN99103401 A CN 99103401A CN 1081091 C CN1081091 C CN 1081091C
- Authority
- CN
- China
- Prior art keywords
- inhibitor
- iron ore
- formaldehyde
- floatation
- antifloating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000003112 inhibitor Substances 0.000 title claims abstract description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title abstract description 56
- 229910052742 iron Inorganic materials 0.000 title abstract description 28
- 238000004519 manufacturing process Methods 0.000 title 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000009833 condensation Methods 0.000 claims abstract description 9
- 230000005494 condensation Effects 0.000 claims abstract description 9
- 229910001608 iron mineral Inorganic materials 0.000 claims abstract description 5
- 239000007859 condensation product Substances 0.000 claims description 11
- 159000000000 sodium salts Chemical class 0.000 claims description 10
- 238000005188 flotation Methods 0.000 claims description 8
- 239000003205 fragrance Substances 0.000 claims description 5
- WODGMMJHSAKKNF-UHFFFAOYSA-N 2-methylnaphthalene-1-sulfonic acid Chemical compound C1=CC=CC2=C(S(O)(=O)=O)C(C)=CC=C21 WODGMMJHSAKKNF-UHFFFAOYSA-N 0.000 claims description 4
- -1 compound sodium salt Chemical class 0.000 claims description 4
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- ISXSFOPKZQZDAO-UHFFFAOYSA-N formaldehyde;sodium Chemical compound [Na].O=C ISXSFOPKZQZDAO-UHFFFAOYSA-N 0.000 claims description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 239000012141 concentrate Substances 0.000 abstract description 7
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 6
- 229920000881 Modified starch Polymers 0.000 abstract description 5
- 239000004368 Modified starch Substances 0.000 abstract description 5
- 235000019426 modified starch Nutrition 0.000 abstract description 5
- 150000001491 aromatic compounds Chemical class 0.000 abstract description 4
- 238000006386 neutralization reaction Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- 238000006277 sulfonation reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000012736 aqueous medium Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical class C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 description 5
- 125000003118 aryl group Chemical group 0.000 description 5
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 4
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 4
- 229920002472 Starch Polymers 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 150000001454 anthracenes Chemical class 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to a preparation method for a reverse-floatation inhibitor of iron minerals. The method comprises the following steps: an aromatic compound, a sulfonating agent (sulfonation), water (an aqueous medium), formaldehyde (condensation), NaOH (neutralization) and products. The inhibitor has good effect; reverse-floatation tests prove that the grade beta and the recovery ratio zeta of iron ore concentrate are higher than the floatation indexes of modified starch; particularly, the present invention is suitable for the floatation of low-grade minerals difficult to float without desliming; and accordingly, the present invention has the advantages of simplifying ore dressing processes, reducing device investment and operation expenses and having obvious economical and social benefits.
Description
The present invention relates to a kind of iron ore antifloating method, belong to chemical material technical field.
For a long time, the reverse flotation inhibitor of iron mineral all adopts modified starch (causticity starch and CMS etc.) both at home and abroad, as the big iron ore of Di Erdeng of the U.S. and China's eight or the five key project Anshan iron and steel plants platform iron ore that assembles troops.In reverse floatation process, add the modified starch inhibitor, after flotation, inhibitor is suppressed at iron mineral in the ore pulp, other impurity come-up is told, and adds the modified starch inhibitor in the impurity of emersion again, behind reverse flotation repeatedly, remove the impurity of emersion, useful mineral matter is stayed in the ore pulp to greatest extent.Assemble troops with regard to the platform ore dressing plant with regard to Anshan iron and steel plant, the annual needs consumes 8000 tons of starch, is equivalent to the city grain of one 300,000 population, populous for one, China that arable area is limited to consume a large amount of grains as the raw material of industry, does not meet China's national situation.
The objective of the invention is to study a kind of preparation method of iron ore antifloating inhibitor, novel iron ore reverse flotation inhibitor with aromatic sulphonic acid formaldehyde condensation products substituting modification starch, it has good dispersiveness and wetability, and especially it is to distinctive high selectivity of iron ore antifloating and strong inhibition.
Obviously, a further object of the invention is, proposes a kind of iron ore antifloating method, replaces inhibitor in the former method with new inhibitor, to save food, tallies with the national condition.
The preparation method of iron ore antifloating inhibitor of the present invention, being divided into was four steps: sulfonation, water Jie, condensation and neutralization.Technical process is:
Aromatic compound-sulfonating agent (sulfonation)-water (water Jie)-formaldehyde (condensation)-NaOH (neutralization)-product.
1, sulfonating reaction
The aromatic compound input is had in the there-necked flask of reflux condenser, thermometer, electric mixing device, heat with oil bath, to 120 ℃-140 ℃ slow sulfonating agents that add of beginning, the mol ratio of addition is: aromatic compound: sulfonating agent=1: 1-3, the limit edged stirs, to 150 ℃-165 ℃, constant temperature 2-3 hour;
2, water medium reaction
Be cooled to below 120 ℃, add water, add sulfonating agent, making total acidity is 25-40%;
3, condensation reaction
Be cooled to below 90 ℃, gradation adds formaldehyde, and the mol ratio of addition is: aromatic compound: formaldehyde=1: 0.5-1.5, be warming up to 90-110 ℃, and constant temperature 2-3 hour, making viscosity was 1 " 31-2 ";
4, neutralization reaction
5, add certain density NaOH solution, addition is aromatic series chemical combination: NaOH=1: 0.8-4, and responseless sulfonating agent is neutralized to neutrality, and makes product be transformed into sodium salt, is inhibitor of the present invention.
Iron ore antifloating method of the present invention, wherein used inhibitor are any in naphthalene sulfonic acid-formaldehyde condensation product sodium salt, condensation compound of methyl naphthalene sulfonic acid and formaldehyde sodium salt, rylnthracene sulfonin formaldehyde condensation products sodium salt or the luxuriant and rich with fragrance sulfonic formaldehyde condensation compound sodium salt.
Inhibitor with method preparation of the present invention, as iron ore antifloating inhibitor, receive good effect, through the reverse flotation test, iron concentrate grade β and rate of recovery ξ are higher than the floatation indicators of modified starch, and especially it is suitable for the flotation of more low-grade refractory minerals and need not desliming, thereby simplified ore-dressing technique, reduced the equipment input, reduced operating cost, its economic benefit and social benefit are extremely remarkable.
Introduce embodiments of the invention below:
Embodiment 1 drops into 128 gram (1 mole) naphthalenes in the there-necked flask, is heated to 130 ℃, slowly adds 98%H
2SO
4128 grams (naphthalene is 1: 1.31 with the ratio of the mole of sulfuric acid), the reinforced time is controlled at more than the 0.5h, and the limit edged stirs, to 160 ℃~165 ℃, constant temperature 2.5h.Be cooled to 120 ℃, add about 40 milliliters in water,, add H
2SO
4Tens grams stir evenly, and making total acidity is 30%.Be cooled to 90 ℃, gradation adds formaldehyde 30 grams (ratio of naphthalene and the mole of formaldehyde 1: 1), and the reinforced time is controlled at 0.5h, heats up 100 ℃ constant temperature 2~3 hours, mensuration viscosity 1 ' 20 ".Add saturated NaOH solution, (about the NaOH36 gram) generates the naphthalene sulfonic acid-formaldehyde condensation product sodium salt, measures nucleome and counts n>9, as iron ore antifloating test, iron ore concentrate index: grade 65.41%, the rate of recovery 89.27%.
Embodiment 2 drops into 142 gram (1 mole) methyl naphthalenes in the there-necked flask, is heated to 130 ℃, slowly adds 98%H
2SO
4137 grams (methyl naphthalene is 1: 1.40 with the ratio of the mole of sulfuric acid), more than the reinforced time control 0.5h, the limit edged stirs, to 160 ℃~165 ℃, constant temperature 2.5h.Lower the temperature 120 ℃, add about 40 milliliters in water, add H
2SO
4Tens grams stir evenly, and survey total acidity 30%.Be cooled to 90 ℃, gradation adds formaldehyde 33 grams (ratio of methyl naphthalene and the mole of formaldehyde 1: 1.1), and the reinforced time is controlled at 0.5h, heats up 100 ℃ constant temperature 2~3 hours, mensuration viscosity 1 ' 5 ".Add saturated NaOH solution (about NaOH 40 grams), generate the condensation compound of methyl naphthalene sulfonic acid and formaldehyde sodium salt, measure nucleome and count n>4, as iron ore antifloating test, iron ore concentrate index: grade 61.98%, the rate of recovery 72.53%.
Embodiment 3 drops into 178 gram (1 mole) anthracenes in the there-necked flask, is heated to 130 ℃, slowly adds 98%H
2SO
4137 grams (anthracene is 1: 1.40 with the ratio of the mole of sulfuric acid), more than the reinforced time control 0.5h, the limit edged stirs, to 160 ℃~165 ℃, constant temperature 2.5h.Lower the temperature 120 ℃, add about 40 milliliters in water, add H
2SO
4Tens grams stir evenly, and survey total acidity 30%.Be cooled to 90 ℃, gradation adds formaldehyde 33 grams (ratio of anthracene and the mole of formaldehyde 1: 1.1), and the reinforced time is controlled at 0.5h, is warming up to 100 ℃, constant temperature 2~3 hours, mensuration viscosity 1 ' 10 ".Add saturated NaOH solution (about NaOH 40 grams), generate rylnthracene sulfonin formaldehyde condensation products sodium salt.As iron ore antifloating test, iron ore concentrate index: grade 61.70%, the rate of recovery 74.62%.
Embodiment 4 is heated to 130 ℃ with in the luxuriant and rich with fragrance input of 178 grams (1 mole) there-necked flask, slowly adds 98%H
2SO
4137 grams (phenanthrene is 1: 1.40 with the ratio of the mole of sulfuric acid), more than the reinforced time control 0.5h, the limit edged stirs, to 160 ℃~165 ℃, constant temperature 2.5h.Lower the temperature 120 ℃, add about 40 milliliters in water, add H
2SO
4Tens grams stir evenly, and survey total acidity 30%.Be cooled to 90 ℃, gradation adds formaldehyde 33 grams (ratio of the mole of luxuriant and rich with fragrance and formaldehyde 1: 1.1), and the reinforced time is controlled at 0.5h, is warming up to 100 ℃, constant temperature 2~3 hours, mensuration viscosity 1 ' 15 ".Add saturated NaOH solution (about NaOH 40 grams), generate luxuriant and rich with fragrance sulfonic formaldehyde condensation compound sodium salt.
Aromatic sulphonic acid formaldehyde condensation products sodium salt can be used alone as the reverse flotation test of iron mineral, also several different aromatic sulphonic acid formaldehyde condensation products sodium salts can be prepared use by a certain percentage, for example the naphthalene sulfonic acid-formaldehyde condensation product sodium salt is 1: 1 with the ratio of methyl naphthalene sulfonic acid condensation product sodium, be used for iron ore antifloating, iron concentrate grade 64.95, yield 88.21%.
Do the iron ore antifloating test with iron ore antifloating inhibitor of the present invention, the grade of iron ore concentrate and the rate of recovery reach the best index of domestic technology respectively.Illustrate that this product is the very superior iron ore antifloating inhibitor of performance.
Claims (1)
1, a kind of reverse flotation method of iron mineral, it is characterized in that inhibitor used in this method is: any in naphthalene sulfonic acid-formaldehyde condensation product sodium salt, condensation compound of methyl naphthalene sulfonic acid and formaldehyde sodium salt, rylnthracene sulfonin formaldehyde condensation products sodium salt or the luxuriant and rich with fragrance sulfonic formaldehyde condensation compound sodium salt.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN99103401A CN1081091C (en) | 1999-03-26 | 1999-03-26 | Process for preparing iron ore antifloating inhibitor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN99103401A CN1081091C (en) | 1999-03-26 | 1999-03-26 | Process for preparing iron ore antifloating inhibitor |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1231219A CN1231219A (en) | 1999-10-13 |
CN1081091C true CN1081091C (en) | 2002-03-20 |
Family
ID=5271257
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CN99103401A Expired - Fee Related CN1081091C (en) | 1999-03-26 | 1999-03-26 | Process for preparing iron ore antifloating inhibitor |
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Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101612610B (en) * | 2009-06-22 | 2012-10-03 | 广西华锡集团股份有限公司 | Preparation method of inhibitor of argillaceous and carbonaceous gangue minerals |
CN103977906B (en) * | 2014-06-09 | 2017-11-17 | 河北钢铁集团矿山设计有限公司 | Reverse flotation ambient-temperature collector and preparation method thereof |
CN104226488B (en) * | 2014-07-29 | 2016-08-03 | 唐山学院 | The preparation method of microfine hematite reverse flotation inhibitor |
CN104437888A (en) * | 2014-11-21 | 2015-03-25 | 广西大学 | Method for preparing zinc-sulfur mineral depressor |
CN106824550B (en) * | 2017-03-22 | 2018-12-04 | 天津天宝翔科技有限公司 | A kind of iron mineral inhibitor and preparation method thereof |
CN108855627A (en) * | 2018-05-18 | 2018-11-23 | 中蓝长化工程科技有限公司 | The composite restrainer and method of iron-bearing mineral in a kind of inhibition Collophanite flotation |
CN108636616B (en) * | 2018-05-22 | 2019-10-08 | 中南大学 | Inhibit the inhibitor and its application method of vulcanization M in a kind of floatation process |
CN113617532B (en) * | 2021-08-09 | 2023-01-24 | 彝良驰宏矿业有限公司 | Combined inhibitor for lead-sulfur sulfide ore flotation separation and application |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS51133102A (en) * | 1975-05-16 | 1976-11-18 | Dowa Mining Co | Flotation method for complicated sulfide mineral |
-
1999
- 1999-03-26 CN CN99103401A patent/CN1081091C/en not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS51133102A (en) * | 1975-05-16 | 1976-11-18 | Dowa Mining Co | Flotation method for complicated sulfide mineral |
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CN1231219A (en) | 1999-10-13 |
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