CN105197941A - Method for preparing high-activity white carbon black through utilizing manganese carbonate leaching residues and electrolytic manganese waste acid - Google Patents
Method for preparing high-activity white carbon black through utilizing manganese carbonate leaching residues and electrolytic manganese waste acid Download PDFInfo
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Abstract
The invention relates to the technical field of recycling and reuse of industrial residues and waste acid, and particularly discloses a method for preparing high-activity white carbon black through utilizing manganese carbonate leaching residues and electrolytic manganese waste acid. The method includes the following steps: washing the manganese carbonate leaching residues directly by tap water to neutral, and then drying; performing microwave processing for 1-5 min on the dried solid powder; reacting the obtained waste activated manganese residues with a strong alkaline solution, and filtering to obtain the filtrate; decolorizing the filtrate through dithiocar-bamate of polyacrylamide with high molecular weight to obtain a silicate aqueous solution; slowly and dropwise adding the decolorized electrolytic manganese waste acid solution; and heating, reacting, filtering, washing and drying to obtain the white carbon block. According to the method provided by the invention, waste residues and waste liquor generated from manganese ore enterprises are effectively utilized to generate high value-added white carbon black, so that environmental protection and comprehensive utilization of resources are facilitated; and the method has the advantages of simple technology, low cost, high added value, high suitability for industrial production, and the like.
Description
Technical field
The present invention relates to the recovery and reuse technology field of industrial residue and spent acid, be specifically related to a kind of method utilizing manganous carbonate leached mud and electrolytic manganese spent acid to prepare high reactivity white carbon black.
Background technology
Manganese produces iron and steel and stainless raw material, and by pulling of Iron and Steel Production sustainable growth, the demand of China to manganese ore constantly rises.China is as mn site doping producing country maximum in the world, and be the country that manganese resource storage enriches very much, but the average grade of manganese ore is lower, the manganese ore reserves in the whole nation 93.6% belong to poor manganese ore.According to statistics, every electrolysis production 1 ton of manganese is by generation 6 ~ 7 tons of manganese leached muds, and along with the acceleration of manganese ore exploitation and the continuous increase of manganese demand, in poor manganese ore, Fe content is fewer and feweri, the waste residue that production manganese produces gets more and more, environmental pollution is on the rise, therefore imperative to the research of the recycling of manganese leached mud.
The relevant report of current domestic manganese leaching residue treating concentrates on mostly prepares the field such as material of construction, 4A molecular sieve, and these techniques all need the operation through high-temperature calcination, and production cost is high, and to obtain value-added content of product lower, essentially no economic benefit; Therefore the development trend that the higher product of manganese leached mud supervene value and production technique thereof will be manganese ore industry Solid state fermentation is utilized.
White carbon black is widely used in rubber, the packing strengthening agent of plastics, ink thickeners, paint additive, the field such as synthetic grease and silicone grease viscosifying agent, curriery flatting agent, pesticide dispersing agent, papermaking weighting agent, the additive of synthetic resins (vibrin, the Elastic polyurethane), electric industry insulation and thermal insulation filler and daily-use chemical industry raw material.High reactivity white carbon black as rubber reinforcing filler can improve vulcanized rubber article tensile strength, hardness, deflect, tear, wear away, ageing-resistant performance, be light color, the colored and indispensable high-quality reinforcing filler of transparent rubber goods, be widely used as the reinforcement of the products such as colored rain boots, sports shoes, translucent Shoe-soles, tire, rubber roll, cable; Strengthening agent as plastics boardy product can improve its solidity to corrosion, weathering resistance and levelling property.Have associated specialist to estimate, under the drive of tire and shoe industry, the speed with annual 8% ~ 10% increases the demand of white carbon black by China fast; Then because particle is less, specific surface area is larger, price is higher for the price of white carbon black.Chinese patent ZL200610035724.5 once reported that active carbon white prepared by the white bauxite waste residue utilizing impurity less, and its silicon-dioxide is mainly used in the rubber materials that tensile strength is less demanding, productive rate is lower.Electrolytic manganese waste residue is prepared in white carbon black process and will be produced the sodium silicate solution of brownish black, in solution, deviating from of nonferrous metal ion is the key obtaining white high-performance white carbon black, the Chinese patent (ZL201010515069.X) of Zhang Daohong report once prepared white carbon black by techniques such as gac, end carboxyl super branched polyester decolourings, wherein dioxide-containing silica is greater than 95%, and specific surface area is greater than 270m
2/ g, but the consumption of end carboxyl super branched polyester is large, and cost is higher; Chinese patent (ZL201110105896.6) with posttension road flood report adopts again gac, amine-terminated hyperbrancedization polyester, polyacrylamide to be discoloring agent, the white carbon black activity of preparation is high, specific surface area is large, but productive rate is on the low side, technique relative complex.
So far there is not yet the report obtaining high, the active high white carbon black of productive rate with the technology that the brown manganous carbonate leached mud that impurity is more is simple by technique, with low cost.Waste acid liquor after electrolytic manganese can not directly discharge because acidic substance concentration is higher, therefore these waste residues of disposal and utilization, waste liquid become more important to environment protection.
Summary of the invention
The technical problem to be solved in the present invention makes full use of the industrial residue of manganese source mill and waste liquid and provides a kind of method utilizing manganous carbonate leached mud and electrolytic manganese spent acid to prepare high reactivity white carbon black.
The present invention solves the problems of the technologies described above with following technical scheme:
Utilize manganous carbonate leached mud and electrolytic manganese spent acid to prepare a method for high reactivity white carbon black, its step is as follows:
1, manganous carbonate leached mud tap water is washed till elutant be neutral after dry, obtain manganese slag, by the microwave treatment 1 ~ 5 minute of manganese slag 800-1200W, obtain refined manganese dioxide waste residue;
2, get the refined manganese dioxide waste residue that step 1 obtains, add the strong base solution that concentration is 40 ~ 45wt%, at 120 ~ 135 DEG C, react 1 ~ 1.5h, filter, and filter residue to be washed till elutant with distilled water be neutral, water lotion is merged in filtrate, collects filtrate;
Wherein strong base solution and step 2 get refined manganese dioxide waste residue mass ratio be 2 ~ 2.5:1;
Described highly basic is sodium hydroxide and/or potassium hydroxide;
3, filtrate step 2 obtained is filtered after decolouring 5 minutes by the dithiocar-bamate of high molecular weight polyacrylamide at 40 ~ 80 DEG C, obtains aqueous silicate solution;
Wherein the dithiocar-bamate of high molecular weight polyacrylamide and step 2 get refined manganese dioxide waste residue weight ratio be 1:1000 ~ 2000, the molecular weight of polyacrylamide is 5,000,000 ~ 10,000,000;
4, get electrolytic manganese spent acid, with the dithiocar-bamate process decolouring in 5 minutes of high molecular weight polyacrylamide at 60 ~ 80 DEG C, obtain faint yellow to colourless aqueous sulfuric acid;
Dithiocar-bamate and the electrolytic manganese spent acid weight ratio of high molecular weight polyacrylamide are 1:1000 ~ 5000.
5, the aqueous silicate solution after the decolouring obtained in step 3 joined in reactor, add the content that water regulates silicon-dioxide in filtrate, the electrolytic manganese spent acid after desolventing technology (i.e. step 4 obtain aqueous sulfuric acid) is slowly dripped under 40 DEG C of agitation conditions, pH value to solution is 5 ~ 8, after dropwising, 0.5 ~ 2h is reacted again at 40 ~ 60 DEG C, then filter, be washed to till can't detect sulfate ion with barium chloride solution, gained precipitated drying and obtains white carbon black;
The water wherein added and step 2 get the weight ratio 2.5 ~ 3.0:1 of refined manganese dioxide waste residue.
Described manganous carbonate leached mud and electrolytic manganese spent acid are the industrial residue that utilizes manganous carbonate and gas washing in SA production manganese metal and produce and spent acid.
The dithiocar-bamate of described high molecular weight polyacrylamide is sodium salt or sylvite.
The preparation method of the dithiocar-bamate of high molecular weight polyacrylamide is: the aqueous solution being 5wt% by the concentration that 1.0mol dithiocarbonic anhydride, 1.0mol highly basic (sodium hydroxide or potassium hydroxide) configure mixes with 100g high molecular weight polyacrylamide powder, stirring reaction 4 hours under 40 DEG C of conditions, then crystallisation by cooling, filtration, drying, namely obtains the dithiocar-bamate pressed powder of high molecular weight polyacrylamide.
Wherein, the molecular weight of high molecular weight polyacrylamide is 5,000,000 ~ 1,000 ten thousand.
Compared with prior art, the advantage of the inventive method and beneficial effect as follows:
(1) the present invention is directly with washing waste residue from the beginning, then uses microwave activation waste residue, and the reaction times of waste residue and strong base solution is significantly lowered, and effectively improves efficiency and saves the energy, can effectively reduce costs and realize industrialization.
(2) the present invention only uses a kind of discoloring agent (dithiocar-bamate of high molecular weight polyacrylamide), and technique is simple, processing ease, and consumption is less, is also conducive to reducing costs.
(3) dithiocar-bamate containing part high molecular weight polyacrylamide in the middle of the Waste Sulfuric Acid after decolouring; the effect of particle promoting agent can be served as; the organic protective layer of one deck is formed on the surface of white carbon black; white carbon black is easily disperseed; particle diameter reduces; specific surface area improves, and the consistency of white carbon black and the polymkeric substance such as rubber, plastics improves, and is conducive to the quality and the added value that improve white carbon black.
(4) white carbon black of the waste residue effectively utilizing manganese ore enterprise to produce and spent acid production high added value, is conducive to the comprehensive utilization of environment protection and resource; And have that technique is simple, with low cost, added value is high, be suitable for suitability for industrialized production.
Embodiment
So far there are no utilizing the dithiocar-bamate of microwave technology and high molecular weight polyacrylamide to realize the report that manganous carbonate leaches slag to prepare high activity white carbon black.The key of technical solution of the present invention is the effective elimination to the foreign pigment such as iron, magnesium, zirconium, chromium contained in manganese leached mud and electrolytic manganese spent acid, and these impurity will directly have influence on quality and the whiteness of white carbon black.The molten impurity of alkali in silicate solutions after the present invention utilizes the dithiocar-bamate of high molecular weight polyacrylamide to deviate from manganese leached mud and alkali reaction, deviate from the acid-soluble impurity in electrolytic manganese spent acid, dithiocar-bamate due to high molecular weight polyacrylamide contains a large amount of carbaminates can effective complexing foreign pigment, can obtain faint yellow to colourless silicate solutions and waste acid liquor, high silicon dioxide content and high-grade white carbon black product could be obtained further.
Secondly, the particle promoting agent that the present invention adopts also is the dithiocar-bamate of high molecular weight polyacrylamide, in-situ modified white carbon black, its surface is enable to connect some particle active groups, form one deck organic protection layer, not only effectively can reduce the free energy on white carbon black surface but also easily disperse, reduce particle diameter, increasing specific surface area, be conducive to dispersion in white carbon black application process and improve and the consistency of rubber, the existence of these organic groups simultaneously makes white carbon black and rubber, the consistency of the polymkeric substance such as plastics improves, be conducive to the quality and the added value that improve white carbon black.
Below in conjunction with specific embodiment, the inventive method is described further, if material used does not have specified otherwise, is then commercially available prod.
The industrial residue that oxide spinel manganese leached mud used in following examples and electrolytic manganese spent acid utilize manganous carbonate and gas washing in SA production manganese metal to produce for Zhongxin Dameng Mining Industry Co., Ltd. and spent acid.
The main component of manganous carbonate leached mud and content are in table 1, and the leading indicator of electrolytic manganese spent acid is in table 2.
The component list of table 1 manganous carbonate leached mud
| Composition | MnO | Al 2O 3 | SiO 2 | Fe 2O 3 | CaO | MgO | H 2O and other |
| Content, wt% | 8-10 | 12-16 | 15-20 | 5-7 | 6-8 | 3-5 | Surplus |
The leading indicator of table 2 electrolytic manganese spent acid
| Composition | pH | Iron level, % | Copper content, % | Aluminium content, % |
| Index | 3-4 | 0.5-1 | 0.1-0.2 | 5-7 |
Embodiment 1
The preparation of the nabam of high molecular weight polyacrylamide:
The Polyacrylamide Powder be the aqueous solution and the 100g molecular weight of 5wt% by the concentration that 1.0mol dithiocarbonic anhydride, 1.0mol sodium hydroxide are configured to being 5,000,000 mixes, stirring reaction 4 hours under 40 DEG C of conditions, then crystallisation by cooling, filtration, drying, obtains the nabam pressed powder 190g of high molecular weight polyacrylamide.
The preparation of high reactivity white carbon black, step is as follows:
(1) it is neutral for 500g manganous carbonate leached mud tap water being washed till elutant, then 120 DEG C of dryings, obtains about 460g manganese slag; Then use 800W microwave treatment 5 minutes, obtain refined manganese dioxide waste residue;
(2) get the refined manganese dioxide waste residue that 100g step (1) obtains, add the sodium hydroxide solution 250g of 40wt%, about 120 DEG C reactions 90 minutes, filter, and filter residue to be washed till elutant with distilled water be neutral, elutant is incorporated into filtrate, collects filtrate;
(3) by step (2) gained filtrate at about 40 DEG C, the nabam adding high molecular weight polyacrylamide prepared by 0.1g the present embodiment stirs 5min desolventing technology, then filter, obtain faint yellow to colourless aqueous silicate solution;
(4) get electrolytic manganese spent acid 1000g, after the nabam of about the 60 DEG C high molecular weight polyacrylamides prepared with 0.2g the present embodiment stirs 5min desolventing technology, obtain faint yellow to colourless aqueous sulfuric acid;
(5) join in reactor by the aqueous silicate solution that step (3) obtains, add water 250g, slowly drips the aqueous sulfuric acid that step (4) obtains under 40 DEG C of agitation conditions, and the pH value to solution is 6.5; Again at about 40 DEG C reaction 2h, till then filtering, being washed to and can't detect sulfate ion with barium chloride solution, gained is deposited in about 120 DEG C dry 5h, obtains white carbon black 16.0g, and after testing, the index of gained white carbon black product is as shown in table 3.
Embodiment 2
The preparation of the dithiocarbamic acid potassium of high molecular weight polyacrylamide:
The Polyacrylamide Powder be the aqueous solution and the 100g molecular weight of 5wt% by the concentration that 1.0mol dithiocarbonic anhydride, 1.0mol potassium hydroxide are configured to being 1,000 ten thousand mixes, stirring reaction 4 hours under 40 DEG C of conditions, then crystallisation by cooling, filtration, drying, obtains the dithiocarbamic acid potassium pressed powder 195g of high molecular weight polyacrylamide.
The preparation of high reactivity white carbon black, step is as follows:
(1) it is neutral for 500g manganous carbonate leached mud tap water being washed till elutant, then 120 DEG C of dryings, obtains about 455g manganese slag; Then use 1000W microwave treatment 3 minutes, obtain refined manganese dioxide waste residue;
(2) get the refined manganese dioxide waste residue that 100g step (1) obtains, add the sodium hydroxide solution 200g of 45wt%, about 135 DEG C reactions 60 minutes, filter, and filter residue to be washed till elutant with distilled water be neutral, elutant is incorporated into filtrate, collects filtrate;
(3) by step (2) gained filtrate at about 60 DEG C, the dithiocarbamic acid potassium adding high molecular weight polyacrylamide prepared by 0.07g the present embodiment stirs 5min desolventing technology, then filter, obtain faint yellow to colourless aqueous silicate solution;
(4) get electrolytic manganese spent acid 1000g, after the dithiocarbamic acid potassium of about the 70 DEG C high molecular weight polyacrylamides prepared with 1.0g the present embodiment stirs 5min desolventing technology, obtain faint yellow to colourless aqueous sulfuric acid;
(5) join in reactor by the aqueous silicate solution that step (3) obtains, add water 270g, slowly drips the aqueous sulfuric acid that step (4) obtains under 40 DEG C of agitation conditions, and the pH value to solution is 6.0; Again at about 60 DEG C reaction 0.5h, till then filtering, being washed to and can't detect sulfate ion with barium chloride solution, gained is deposited in about 120 DEG C dry 5h, obtains white carbon black 16.2g, and after testing, the index of gained white carbon black product is as shown in table 3.
Embodiment 3
The preparation of the dithiocarbamic acid potassium of high molecular weight polyacrylamide:
The Polyacrylamide Powder be the aqueous solution and the 100g molecular weight of 5wt% by the concentration that 1.0mol dithiocarbonic anhydride, 1.0mol potassium hydroxide are configured to being 5,000,000 mixes, stirring reaction 4 hours under 40 DEG C of conditions, then crystallisation by cooling, filtration, drying, obtains the dithiocarbamic acid potassium pressed powder 197g of high molecular weight polyacrylamide.
The preparation of high reactivity white carbon black, step is as follows:
(1) it is neutral for 500g manganous carbonate leached mud tap water being washed till elutant, then 120 DEG C of dryings, obtains about 465g manganese slag; Then use 1200W microwave treatment 1 minute, obtain refined manganese dioxide waste residue;
(2) get the refined manganese dioxide waste residue that 100g step (1) obtains, add the sodium hydroxide solution 220g of 42wt%, about 130 DEG C reactions 75 minutes, filter, and filter residue to be washed till elutant with distilled water be neutral, elutant is incorporated into filtrate, collects filtrate;
(3) by step (2) gained filtrate at about 80 DEG C, the dithiocarbamic acid potassium adding high molecular weight polyacrylamide prepared by 0.05g the present embodiment stirs 5min desolventing technology, then filter, obtain faint yellow to colourless aqueous silicate solution;
(4) get electrolytic manganese spent acid 1000g, after the dithiocarbamic acid potassium of about the 80 DEG C high molecular weight polyacrylamides prepared with 0.5g the present embodiment stirs 5min desolventing technology, obtain faint yellow to colourless aqueous sulfuric acid;
(5) join in reactor by the aqueous silicate solution that step (3) obtains, add water 300g, slowly drips the aqueous sulfuric acid that step (4) obtains under 40 DEG C of agitation conditions, and the pH value to solution is 5.0; Again at about 50 DEG C reaction 1.5h, till then filtering, being washed to and can't detect sulfate ion with barium chloride solution, gained is deposited in about 120 DEG C dry 5h, obtains white carbon black 15.8g, and after testing, the index of gained white carbon black product is as shown in table 3.
Embodiment 4
The preparation of the dithiocarbamic acid potassium of high molecular weight polyacrylamide:
The Polyacrylamide Powder be the aqueous solution and the 100g molecular weight of 5wt% by the concentration that 1.0mol dithiocarbonic anhydride, 1.0mol potassium hydroxide are configured to being 1,000 ten thousand mixes, stirring reaction 4 hours under 40 DEG C of conditions, then crystallisation by cooling, filtration, drying, obtains the dithiocarbamic acid potassium pressed powder 198g of high molecular weight polyacrylamide.
The preparation of high reactivity white carbon black, step is as follows:
(1) it is neutral for 500g manganous carbonate leached mud tap water being washed till elutant, then 120 DEG C of dryings, obtains about 470g manganese slag; Then use 1000W microwave treatment 4 minutes, obtain refined manganese dioxide waste residue;
(2) get the refined manganese dioxide waste residue that 100g step (1) obtains, add the potassium hydroxide solution 200g of 42wt%, about 130 DEG C reactions 75 minutes, filter, and filter residue to be washed till elutant with distilled water be neutral, elutant is incorporated into filtrate, collects filtrate;
(3) by step (2) gained filtrate at about 80 DEG C, the dithiocarbamic acid potassium adding high molecular weight polyacrylamide prepared by 0.10g the present embodiment stirs 5min desolventing technology, then filter, obtain faint yellow to colourless aqueous silicate solution;
(4) get electrolytic manganese spent acid 1000g, after the dithiocarbamic acid potassium of about the 70 DEG C high molecular weight polyacrylamides prepared with 0.6g the present embodiment stirs 5min desolventing technology, obtain faint yellow to colourless aqueous sulfuric acid;
(5) join in reactor by the aqueous silicate solution that step (3) obtains, add water 280g, slowly drips the aqueous sulfuric acid that step (4) obtains under 40 DEG C of agitation conditions, and the pH value to solution is 7.5; Again at about 50 DEG C reaction 1.0h, till then filtering, being washed to and can't detect sulfate ion with barium chloride solution, gained is deposited in about 120 DEG C dry 5h, obtains white carbon black 16.5g, and after testing, the index of gained white carbon black product is as shown in table 3.
The performance index of the high reactivity white carbon black that embodiment 1 to embodiment 4 is obtained compare see table 3, and all test indexs are all carried out according to corresponding industry standard or national standard.
Table 3
Above embodiment is to invention has been detailed description; its object is to enable those skilled in the art understand content of the present invention and be implemented; but can not limit the scope of the invention with this; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed in protection scope of the present invention.
Claims (6)
1. utilize manganous carbonate leached mud and electrolytic manganese spent acid to prepare a method for high reactivity white carbon black, its step is as follows:
(1), by manganous carbonate leached mud tap water be washed till elutant be neutral after dry, obtain manganese slag, by the microwave treatment 1 ~ 5 minute of manganese slag 800-1200W, obtain refined manganese dioxide waste residue;
(2), get the refined manganese dioxide waste residue that step (1) obtains, add the strong base solution that concentration is 40 ~ 45wt%, at 120 ~ 135 DEG C, react 1 ~ 1.5h, filter, it is neutral for distilled water, filter residue being washed till elutant, is merged into by water lotion in filtrate, collects filtrate;
Described highly basic is sodium hydroxide and/or potassium hydroxide;
(3) filtrate, by step (2) obtained is filtered with after the dithiocar-bamate decolouring of high molecular weight polyacrylamide at 40 ~ 80 DEG C, obtains aqueous silicate solution;
(4), get electrolytic manganese spent acid, decolour by the dithiocar-bamate of high molecular weight polyacrylamide at 60 ~ 80 DEG C, obtain faint yellow to colourless aqueous sulfuric acid;
The molecular weight of described high molecular weight polyacrylamide is 5,000,000 ~ 1,000 ten thousand;
The dithiocar-bamate of described high molecular weight polyacrylamide is sodium salt or sylvite;
(5), the aqueous silicate solution after the decolouring obtained in step (3) joined in reactor, add the content that water regulates silicon-dioxide in filtrate, the aqueous sulfuric acid that step (4) obtains slowly is dripped under 40 DEG C of agitation conditions, pH value to solution is 5 ~ 8, after dropwising, 0.5 ~ 2h is reacted again at 40 ~ 60 DEG C, then filter, be washed to till can't detect sulfate ion with barium chloride solution, gained precipitated drying and obtains white carbon black.
2. method according to claim 1, it is characterized in that, the preparation method of the dithiocar-bamate of described high molecular weight polyacrylamide is: be that the aqueous solution of 5wt% mixes with 100g high molecular weight polyacrylamide powder by 1.0mol dithiocarbonic anhydride, the concentration that configured by 1.0mol sodium hydroxide or potassium hydroxide, stirring reaction 4 hours under 40 DEG C of conditions, then crystallisation by cooling, filtration, drying, namely obtains the dithiocar-bamate pressed powder of high molecular weight polyacrylamide;
The molecular weight of described high molecular weight polyacrylamide is 5,000,000 ~ 1,000 ten thousand.
3. method according to claim 1 and 2, is characterized in that: in step (2) 40 ~ 45wt% strong base solution and step (2) get refined manganese dioxide waste residue mass ratio be 2 ~ 2.5:1.
4. method according to claim 1 and 2, is characterized in that: in step (3) dithiocar-bamate of high molecular weight polyacrylamide and step (2) get refined manganese dioxide waste residue weight ratio be 1:1000 ~ 2000.
5. method according to claim 1 and 2, is characterized in that: dithiocar-bamate and the electrolytic manganese spent acid weight ratio of the middle high molecular weight polyacrylamide of step (4) are 1:1000 ~ 5000.
6. method according to claim 1 and 2, is characterized in that: the water wherein added in step (5) and step (2) get the weight ratio 2.5 ~ 3.0:1 of refined manganese dioxide waste residue.
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| CN111498864A (en) * | 2020-04-29 | 2020-08-07 | 河南科技大学 | Magnetic zeolite material and preparation method and application thereof |
| CN111498864B (en) * | 2020-04-29 | 2021-11-23 | 河南科技大学 | Magnetic zeolite material and preparation method and application thereof |
| CN111847518A (en) * | 2020-06-28 | 2020-10-30 | 广西锰华新能源科技发展有限公司 | Efficient recycling method of silicomanganese slag |
| CN112441621A (en) * | 2020-11-24 | 2021-03-05 | 鄂尔多斯应用技术学院 | Comprehensive utilization method of manganese-rich slag |
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