CN102443071B - Composite modified starch as hematite reverse flotation inhibitor and preparation method thereof - Google Patents

Composite modified starch as hematite reverse flotation inhibitor and preparation method thereof Download PDF

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Publication number
CN102443071B
CN102443071B CN201110362410.7A CN201110362410A CN102443071B CN 102443071 B CN102443071 B CN 102443071B CN 201110362410 A CN201110362410 A CN 201110362410A CN 102443071 B CN102443071 B CN 102443071B
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composite modified
modified starch
starch
reverse flotation
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CN102443071A (en
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张友全
谢新玲
刘洁
玉琼广
梁露峰
刘绍秀
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GUANGXI STATE FARMS MINGYANG BIOCHEMICAL GROUP Inc
Guangxi University
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GUANGXI STATE FARMS MINGYANG BIOCHEMICAL GROUP Inc
Guangxi University
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Abstract

The invention discloses a kind of composite modified starch as hematite reverse flotation inhibitor and preparation method thereof, its product is by raw starch, clorox is oxygenant, S-WAT and Sodium Nitrite are esterifying agent, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt is cationic reagent, caustic alkali is that catalyzer and water are made, its proportioning is counted by weight: raw starch 100 parts, clorox 0.5 ~ 10 part, S-WAT 1.2 ~ 7.0 parts, Sodium Nitrite 0.2 ~ 1.2 part, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt 0.5 ~ 3.5 part, 3.0 ~ 7.0 parts, caustic alkali, 25 ~ 40 parts, water.Product composite modified starch comprises carboxylate radical, azochlorosulfonate acid anion and quaternary ammonium group positively charged ion, has cold water solubles, low viscosity, the advantages such as the productive rate that can increase hematite concentrates and the filtration condition that improves iron ore concentrate slurry.

Description

Composite modified starch as hematite reverse flotation inhibitor and preparation method thereof
Technical field
The invention belongs to reverse floatation agent preparing technical field in flotation engineering, particularly relate to composite modified starch as hematite reverse flotation inhibitor and preparation method thereof.
Background technology
Rhombohedral iron ore is a kind of oxidized form ore deposit formed under oxidative conditions, and it is mainly composed and is stored in appositional pattern, weathering woods filter type and part by metamorphic sedimentary type, iron ore relevant to volcano-intruder operations.The reserves of China's rhombohedral iron ore have now been verified and have been accounted for 18.1% of national iron ore total reserves, have poor, assorted, thin, associated minerals ratio high.According to statistics, China's red iron iron ore average grade 31.27%, compare with Australia, Brazilian import resources, China's Iron Concentrate Quality still has obvious gap.Such as, Australia mostly is red iron rich ore, fine ore grade 62%, lump ore grade 64%, SiO 2content 3% ~ 4%; Brazil's also mainly red iron rich ore, ore deposit grade 65% ~ 66%, lump ore grade 66% ~ 67%, SiO 2content 1% ~ 2%.Therefore, improving iron ore grade further, reduce foreign matter content, is still the vital task that mineral processing in China worker faces.From raising Iron Concentrate Quality angle, anion reverse floatation technique serves huge effect.Anshan iron and steel plant Qidashan iron ore is the maximum Iron concentrator of China, year process head grade is the rhombohedral iron ore 8,000,000 tons of 29%, and adopted weight-magnetic-direct floatation process before calendar year 2001, concentrate grade reaches 63%, and after 2002, use weight-magnetic-reverse floatation process instead, concentrate grade reaches more than 67.4%.
In hematite reverse flotation technique, W-Gum is the Exemplary inhibitors of iron oxide ore.The ultimate principle of common starch suppression rhombohedral iron ore is: starch is after rhombohedral iron ore surface adsorption, many hydrophilic functional groups that starch itself exists form hydrophilic layer on rhombohedral iron ore thing surface, the surface reaction forces of collecting agent and rhombohedral iron ore grain can be weakened, intercept rhombohedral iron ore grain to be combined with flotation bubble, reduce the flotability of rhombohedral iron ore, thus restraining effect is produced to rhombohedral iron ore.But between rhombohedral iron ore thing and gangue mineral, both surface physicses and chemical property have certain difference, but also there are some similar features, therefore, by common starch as inhibitor time, its suppress selectivity be subject to a definite limitation.
In order to improve the selectivity of starch inhibitor, investigator is had once to propose the inhibitor adopting modified modified starch as rhombohedral iron ore.Also there are some researches show, when with cationic starch as rhombohedral iron ore inhibitor time, in the scope of pH=7 ~ 11, quartz wait gangue than rhombohedral iron ore with more negative charge, cationic starch is 3 times of rhombohedral iron ore in the absorption on quartz mineral surface, and the absorption of anionic starch on rhombohedral iron ore is than much bigger on quartz.Therefore, in reverse floatation process, select anionic starch effectively can improve the selectivity of inhibitor.As, number of patent application 200610124741.6 discloses a kind of beneficiation method of roe shape high-phosphorus hematite, adopt sulfonated starch to suppress roe shape high-phosphorus hematite, by reverse flotation, the impurity such as phosphorus, silicon is removed, the iron ore concentrate that acquisition Iron grade more than 63%, iron recovery are greater than 75%.
But, when using the anionic starch such as sulfonate radical or carboxylate radical as inhibitor, still there is following problem: (1) starch viscosity is high, causing boiling operation and Cemented filling difficulty; (2) contain the assorted positively charged ions such as some calcium, manganese, iron in flotation system, have necessarily " neutralization " to act on to the negatively charged ion in starch, reduce the result of use of anionic starch; (3) along with iron ore fine grinding degree is more and more higher, add that ore pulp itself has higher viscosity, iron concentrate filtering difficulty is still difficult to solve.
Summary of the invention
The object of the invention is to solve the deficiency in above-mentioned technology, a kind of composite modified starch as hematite reverse flotation inhibitor and preparation method thereof is provided, this composite modified starch cold water solubles, low viscosity, can increase the productive rate of hematite concentrates and improve the filtration condition of iron ore concentrate slurry.
To achieve these goals, the technical solution used in the present invention is:
A kind of composite modified starch as hematite reverse flotation inhibitor, be raw material by starch, clorox is oxygenant, S-WAT and Sodium Nitrite are esterifying agent, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt is cationic reagent, caustic alkali is that catalyzer and water are made, its proportioning is counted by weight: raw starch 100 parts, clorox 0.5 ~ 10 part, S-WAT 1.2 ~ 7.0 parts, Sodium Nitrite 0.2 ~ 1.2 part, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt 0.5 ~ 3.5 part, 3.0 ~ 7.0 parts, caustic alkali, 25 ~ 40 parts, water.
Described starch to be selected from tapioca (flour) and W-Gum any one.
Described caustic alkali to be selected from sodium hydroxide and potassium hydroxide any one.
A preparation method for composite modified starch as hematite reverse flotation inhibitor, comprises the steps:
(1) mixing of materials: by starch 100 parts, clorox 0.5 ~ 10 part, S-WAT 1.2 ~ 7.0 parts, Sodium Nitrite 0.2 ~ 1.2 part, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt 0.5 ~ 3.5 part, 3.0 ~ 7.0 parts, caustic alkali and 25 ~ 40 parts, water add mixing tank, are uniformly mixed 1 ~ 3 hour;
(2) extruding reaction: adopt twin-screw extruder to carry out extruding reaction 2 ~ 10 minutes to mixed material, reaction comprises oxidation, esterification and etherification reaction;
(3) aftertreatment: reacted product is cooled to room temperature, pulverizes, by 100 mesh sieves, namely obtains product.
The rotating speed that described mixing tank stirs is 50 ~ 200 r/min.
The working parameter of described twin-screw extruder is: screw slenderness ratio 25, the compression ratio 3.0 of twin screw, screw speed 50 ~ 250 r/min, front-end temperature is 50 ~ 80 DEG C, stage casing temperature is 130 ~ 170 DEG C, and rear temperature is 190 ~ 240 DEG C, extrusion positive pressure 2.0 ~ 3.5MPa.
Its product composite modified starch is in white or micro-yellow powder shape, comprise carboxylate radical, azochlorosulfonate acid anion and quaternary ammonium group positively charged ion, cold water solubles, viscosity is 5 ~ 35mPa.s(6%, 95 DEG C), carboxyl (-COOH) quality percentage is 0.012% ~ 0.3%, and the quality percentage of sulphur (S) is 0.18% ~ 2.0%, and the quality percentage of nitrogen (N) is 0.02% ~ 0.25%.
Compared with prior art, beneficial effect of the present invention is as follows:
The present invention is by extrusion technique, and prepare a kind of cold water solubles through single step reaction, low viscosity, the composite modified starch containing carboxylate radical, azochlorosulfonate acid anion group and quaternary ammonium group cation group, this product has following characteristics:
(1) repel the assorted positively charged ion such as calcium, iron in ore pulp, protection carboxylate radical, azochlorosulfonate acid anion group, adsorb hematite selectively;
(2) the poly-effect of wadding can be played to superfine hematite, the productive rate of hematite concentrates can be increased and improve the filtration condition of iron ore concentrate slurry;
(3) cold water solubles, viscosity is low, eliminates cooking process during use, and Flows is good, solves the problem of blocking pipe.
Namely this product is applicable to anionic collector reverse floatation process, is also applicable to cation-collecting agent reverse floatation process.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to the scope that embodiment represents.
Embodiment 1
Get tapioca (flour) 100 parts, clorox 0.5 part, S-WAT 1.2 parts, Sodium Nitrite 0.2 part, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt 0.5 part, 25 parts, water, 3 parts, sodium hydroxide, add mixing tank, be uniformly mixed 1 hour, controlling extruding puffing front-end temperature is 50 DEG C, and stage casing temperature is 130 DEG C, rear temperature is 190 DEG C, by the material feeding extrusion machine that mixes above with screw speed 250 r/min extruding reaction 2 minutes.
The product carboxyl (-COOH) quality percentage that the present embodiment obtains is 0.01%, and the quality percentage of sulphur (S) is 0.25%, and the quality percentage of nitrogen (N) is 0.026%, and viscosity is 22mPas(6%, 95 DEG C), the composite modified starch product of cold water solubles.This product is 0.8kg/t as rhombohedral iron ore inhibitor at addition, be the rhombohedral iron ore of 43.5% to Iron grade after heavy-magnetic separation, after lime activation, adopt oleic acid lipid acid to open a way reverse flotation to rhombohedral iron ore as collecting agent, obtain that Iron grade is 67.8%, the rate of recovery is the iron ore concentrate of 83.5%.
Embodiment 2
Extracting corn starch 100 parts, clorox 3.0 parts, S-WAT 5.5 parts, Sodium Nitrite 1.0 parts, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt 0.8 part, 25 parts, water, 6 parts, potassium hydroxide, mixes 2 hours in a mixer, controlling extruding puffing front-end temperature is 70 DEG C, stage casing temperature is 155 DEG C, and rear temperature is 220 DEG C, by the material feeding extrusion machine that mixes above with screw speed 125 r/min extruding reaction 5 minutes.
The product carboxyl (-COOH) quality percentage that the present embodiment obtains is 0.024%, and the quality percentage of sulphur (S) is 0.91%, and the quality percentage of nitrogen (N) is 0.052%., viscosity is 13mPas(6%, 95 DEG C), the composite modified starch product of cold water solubles.This product is 0.8kg/t as rhombohedral iron ore inhibitor at addition, be the rhombohedral iron ore of 43.5% to Iron grade after heavy-magnetic separation, after lime activation, adopt oleic acid lipid acid to open a way reverse flotation to rhombohedral iron ore as collecting agent, obtain the iron ore concentrate of Iron grade >68.6%, rate of recovery >86.5%.
Embodiment 3
Get tapioca (flour) 100 parts, clorox 10 parts, S-WAT 7.0 parts, Sodium Nitrite 1.2 parts, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt 3.5 parts, 40 parts, water, 3.5 parts, sodium hydroxide, add mixing tank, be uniformly mixed 3 hours, controlling extruding puffing front-end temperature is 80 DEG C, and stage casing temperature is 170 DEG C, rear temperature is 240 DEG C, by the material feeding extrusion machine that mixes above with screw speed 50 r/min extruding reaction 10 minutes.
The product carboxyl (-COOH) quality percentage that the present embodiment obtains is 0.17%, and the quality percentage of sulphur (S) is 1.35%, and the quality percentage of nitrogen (N) is 0.175%, and viscosity is 8 mPas(6%, 95 DEG C), the composite modified starch product of cold water solubles.This product is 0.8kg/t as rhombohedral iron ore inhibitor at addition, be the rhombohedral iron ore of 43.5% to Iron grade after heavy-magnetic separation, after lime activation, adopt oleic acid lipid acid to open a way reverse flotation to rhombohedral iron ore as collecting agent, obtain that Iron grade is 68.3%, the rate of recovery is the iron ore concentrate of 85.5%.

Claims (8)

1. a composite modified starch as hematite reverse flotation inhibitor, it is characterized in that: be raw material by starch, clorox is oxygenant, S-WAT and Sodium Nitrite are esterifying agent, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt is cationic reagent, caustic alkali is that catalyzer and water are made, its proportioning is counted by weight: raw starch 100 parts, clorox 0.5 ~ 10 part, S-WAT 1.2 ~ 7.0 parts, Sodium Nitrite 0.2 ~ 1.2 part, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt 0.5 ~ 3.5 part, 3.0 ~ 7.0 parts, caustic alkali, 25 ~ 40 parts, water;
Its preparation method comprises the steps:
(1) mixing of materials: by starch 100 parts, clorox 0.5 ~ 10 part, S-WAT 1.2 ~ 7.0 parts, Sodium Nitrite 0.2 ~ 1.2 part, 3-chloro-2-hydroxypropyl trimethylammonium based quaternary ammonium salt 0.5 ~ 3.5 part, 3.0 ~ 7.0 parts, caustic alkali and 25 ~ 40 parts, water add mixing tank, are uniformly mixed 1 ~ 3 hour;
(2) extruding reaction: adopt twin-screw extruder to carry out extruding reaction 2 ~ 10 minutes to mixed material, reaction comprises oxidation, esterification and etherification reaction;
(3) aftertreatment: reacted product is cooled to room temperature, pulverizes, by 100 mesh sieves, namely obtains product.
2. composite modified starch as hematite reverse flotation inhibitor according to claim 1, is characterized in that: described starch to be selected from tapioca (flour) and W-Gum any one.
3. composite modified starch as hematite reverse flotation inhibitor according to claim 1, is characterized in that: described caustic alkali to be selected from sodium hydroxide and potassium hydroxide any one.
4. composite modified starch as hematite reverse flotation inhibitor according to claim 1, is characterized in that: product comprises carboxylate radical, azochlorosulfonate acid anion and quaternary ammonium group positively charged ion.
5. composite modified starch as hematite reverse flotation inhibitor according to claim 1, is characterized in that: the quality percentage of-COOH quality percentage of product to be the quality percentage of 0.012% ~ 0.3%, S be 0.18% ~ 2.0%, N is 0.02% ~ 0.25%.
6. composite modified starch as hematite reverse flotation inhibitor according to claim 1, is characterized in that: product cold water solubles, is 6% in mass percent, and under temperature 95 DEG C of conditions, viscosity is 5 ~ 35mPas.
7. composite modified starch as hematite reverse flotation inhibitor according to claim 1, is characterized in that: the rotating speed that described mixing tank stirs is 50 ~ 200 r/min.
8. composite modified starch as hematite reverse flotation inhibitor according to claim 1, it is characterized in that the working parameter of described twin-screw extruder is: screw slenderness ratio 25, the compression ratio 3.0 of twin screw, screw speed 50 ~ 250 r/min, front-end temperature is 50 ~ 80 DEG C, stage casing temperature is 130 ~ 170 DEG C, and rear temperature is 190 ~ 240 DEG C, extrusion positive pressure 2.0 ~ 3.5MPa.
CN201110362410.7A 2011-11-16 2011-11-16 Composite modified starch as hematite reverse flotation inhibitor and preparation method thereof Expired - Fee Related CN102443071B (en)

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