CN103130230B - Technique for producing white carbon black from silicon rubber pyrolysis ash - Google Patents
Technique for producing white carbon black from silicon rubber pyrolysis ash Download PDFInfo
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- CN103130230B CN103130230B CN201310077903.5A CN201310077903A CN103130230B CN 103130230 B CN103130230 B CN 103130230B CN 201310077903 A CN201310077903 A CN 201310077903A CN 103130230 B CN103130230 B CN 103130230B
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- carbon black
- silicon rubber
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Abstract
The invention relates to a technique for producing white carbon black from silicon rubber pyrolysis ash, belonging to the technical field of chemical engineering. The technique is characterized by comprising the following steps: putting silicon rubber pyrolysis ash in a storage tank, removing inorganic salts with spent acid, putting into a dilute acid reaction tank to react with hydrochloric acid, and putting the ash subjected to pressure filtration into a high-temperature roasting furnace system to remove organic substances by oxidation; and finally, cooling, pulverizing by ball milling, and packaging to obtain the white carbon black. The SiO2 content in the white carbon black is 91-94 wt%. The new technique for recycling silicon rubber pyrolysis ash creatively produces the white carbon black product from the silicon rubber pyrolysis ash by pretreatment-high temperature incineration, and has the characteristics of high technical content and controllable pollution. The invention has great possibility for popularization, and has wide application prospects and obvious economic and environmental benefits.
Description
Technical field
The present invention relates to the technique that a kind of silicon rubber pyrolysis lime-ash produces white carbon black, belong to chemical technology field.
Background technology
China is silicon rubber production, import and consumption big country, and silicon rubber regeneration can save a large amount of petroleum resources and the energy.A large amount of silicon rubber lime-ash is produced in silicon rubber regenerative process, silicon rubber pyrolysis lime-ash is that useless silicon rubber extracts the solid waste after crude oil through high-temperature catalytic thermo-cracking, China produces tens thousand of tons of silicon rubber lime-ash every year, dangerous solid waste is classified as by country, as can not the utilization of resources, the more energy and Disposal sites will be consumed.
Summary of the invention
The object of the invention is for above-mentioned the deficiencies in the prior art, provide a kind of silicon rubber pyrolysis lime-ash to produce the technique of white carbon black.
The object of the invention is to be achieved through the following technical solutions: a kind of silicon rubber pyrolysis lime-ash produces the technique of white carbon black, it is characterized in that, comprises the following steps:
1) silicon rubber pyrolysis lime-ash being put into material stock pond utilizes the spent acid through reaction tentatively to remove inorganic salts material; The spent acid filtered out enters sewage works process in factory after neutralization;
2) fully mix putting into diluted acid reaction tank through spent acid reacted silicon rubber pyrolysis lime-ash in step 1) with dilute hydrochloric acid, reaction 12h, make inorganic metal ion contained in silicon rubber pyrolysis lime-ash be dissolved in dilute hydrochloric acid, remove inorganic salts material, obtain solidliquid mixture; Described diluted acid reaction tank is enamel reactor;
3) by step 2) in solidliquid mixture in plate-and-frame filter press, carry out solid-liquid separation, the liquid separated is spent acid, and spent acid recycling is carried out in material stock pond spent acid being put into step 1); Described plate-and-frame filter press adopts acidproof filter cloth;
4) the silicon rubber pyrolysis lime-ash after press filtration in step 3) is put into that high-temperature roasting furnace system carries out drying, high-temperature calcination, introducing air simultaneously, form oxidation atmosphere, oxidation removal organism, obtains white carbon black powder; Described high-temperature roasting furnace system is made up of oxygen device logical in rotary kiln, kiln, dual firing chamber, flue gas dust-removing desulfurizing device, quencher, producer gas generator and burner;
5) ball mill pulverizing, packing is utilized after the white carbon black powder of step 4) gained being carried out cooling down, obtained white carbon black; SiO in described white carbon black
2content is the 91-94% of gross weight.
In silicon rubber pyrolysis lime-ash main component be silicon, the metal species inorganics such as semicoke (organism) and some iron calcium aluminium that formed in the incomplete organism of pyrolysis or pyrolytic process, technical problem underlying is that inorganic salts removes and organic matter removal, and the silicon compound obtained generates white carbon black after high temperature oxidation.Diluted hydrochloric acid dissolution is adopted to remove lime-ash based on the inorganic salts of Fe salt, Ca salt, Al salt in the present invention, after removing lime-ash inorganic salt, high temperature sintering is carried out to it, oxidation removal organism, in calcination process, introducing air, form oxidation atmosphere, silicon class substance oxidation generates white carbon black (SiO2).
The silicon rubber pyrolysis cinder resource of the present invention's research and development utilizes novel process, is to adopt pre-treatment-high temperature incineration to produce white carbon black product silicon rubber pyrolysis lime-ash first in industry, and the content that possesses skills is high, pollute controlled feature.First silicon rubber pyrolysis lime-ash enters material stock pond spent acid and removes part inorganic salts material, enter diluted acid reaction tank (enamel reactor) afterwards fully to mix with fresh hydrochloric acid, abundant reaction 12h, effect is that inorganic metal ion contained in lime-ash is dissolved in hydrochloric acid, in plate-and-frame filter press, carry out solid-liquid separation, isolated spent acid enters material stock pond and carries out spent acid utilization.Spent acid is after utilizing at this, and acidity is very low (pH is about 3-4), after neutralization, enter sewage works process in factory.The drying system that solid after press filtration enters kiln is dried, and carries out high-temperature calcination after oven dry in rotary kiln, namely obtains white carbon black product afterwards after cooling crush.
A kind of silicon rubber pyrolysis lime-ash that the present invention proposes produces the technique of white carbon black, and the possibility applied is large, has wide practical use, economic benefit, obvious environment benefit.The present invention is the physical and chemical composition based on silicon rubber pyrolysis lime-ash, removes after inorganic salts wherein, high temperature sintering obtain white carbon black (SiO through dilute hydrochloric acid
2content is greater than 90%) product, quality product reaches " rubber ingredients precipitated hydrated silica " (HG/T 3061-2009) chemical industry standard that Ministry of Industry and Information issues.
The white carbon black that the present invention obtains is through adopting " mensuration of precipitated hydrated silica dry sample dioxide-containing silica " (HG/T 3062) methods analyst dioxide-containing silica, the analytical data of 6 batches shows, the dioxide-containing silica of the white carbon black that silicon rubber pyrolysis lime-ash obtains after dilute hydrochloric acid pre-treatment, high temperature sintering, between 91-94%, reaches dioxide-containing silica requirement in " rubber ingredients precipitated hydrated silica " (HG/T 3061-2009) chemical industry standard.By analysis, be mainly in remaining 6-9% composition and be wrapped in not by the inorganic salts of dilute hydrochloric acid stripping in lime-ash particulate, after high temperature sintering, solidify in white carbon black particulate.When this product uses as stopping composition, can not separate out, therefore the white carbon black that the present invention obtains has environmental protection feature.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Silicon rubber pyrolysis lime-ash produces a technique for white carbon black, comprises the following steps:
1) solid waste-silicon rubber pyrolysis lime-ash from production plant being put into material stock pond utilizes the spent acid (the reacted spent acid of later process diluted acid reaction tank, uses spent acid further) through reaction tentatively to remove inorganic salts material; Material stock pond is two alternations, and spent acid becomes spent acid after reacting in material stock pond, is filtered out by spent acid and enter sewage works process in factory after neutralization;
2) fully mix putting into diluted acid reaction tank through spent acid reacted silicon rubber pyrolysis lime-ash in step 1) with dilute hydrochloric acid, reaction 12h, make inorganic metal ion contained in silicon rubber pyrolysis lime-ash be dissolved in dilute hydrochloric acid, remove inorganic salts material, obtain solidliquid mixture; Described diluted acid reaction tank is enamel reactor; Alkene hydrochloric acid in diluted acid reaction tank utilizes acid proof pump to extract from fresh acid storage pond; Inorganic salts is Fe salt, Ca salt, Al salt;
3) by step 2) in solidliquid mixture in plate-and-frame filter press, carry out solid-liquid separation, the liquid separated is spent acid, and spent acid recycling is carried out in material stock pond spent acid being put into step 1); Described plate-and-frame filter press adopts acidproof filter cloth;
4) the silicon rubber pyrolysis lime-ash after press filtration in step 3) is put into that high-temperature roasting furnace system carries out drying, high-temperature calcination, dust-removal and desulfurizing, simultaneously introducing air, form oxidation atmosphere, oxidation removal organism, obtains white carbon black powder simultaneously; Described high-temperature roasting furnace system is made up of oxygen device logical in rotary kiln, kiln, dual firing chamber, flue gas dust-removing desulfurizing device, quencher, producer gas generator and burner;
5) white carbon black powder of step 4) gained is put into cooling kiln carry out cooling down after and utilize ball mill pulverizing, packing, obtained white carbon black; SiO in described white carbon black
2content is the 91-94% of gross weight, and the 6-9% of residue gross weight is wrapped in not by the inorganic salts of hydrochloric acid stripping in silicon rubber pyrolysis lime-ash particulate, and this part inorganic salts, after high-temperature roasting, solidifies in white carbon black particulate.
Claims (1)
1. produce the technique of white carbon black with silicon rubber pyrolysis lime-ash for one kind, comprise and utilize high-temperature roasting furnace system to carry out high-temperature calcination, and to cooled material ball mill pulverizing, packing, described high-temperature roasting furnace system is made up of oxygen device logical in rotary kiln, kiln, dual firing chamber, flue gas dust-removing desulfurizing device, quencher, producer gas generator and burner, it is characterized in that, comprise the following steps:
1) solid waste-silicon rubber pyrolysis lime-ash from production plant being put into material stock pond utilizes the spent acid through reaction tentatively to remove inorganic salts material; Material stock pond is two alternations, and spent acid becomes spent acid after reacting in material stock pond, and the spent acid filtered out enters sewage works process in factory after neutralization;
2) by step 1) in put into diluted acid reaction tank through spent acid reacted silicon rubber pyrolysis lime-ash and fully mix with dilute hydrochloric acid, reaction 12h, make inorganic metal ion contained in silicon rubber pyrolysis lime-ash be dissolved in dilute hydrochloric acid, remove inorganic salts material, obtain solidliquid mixture; Described diluted acid reaction tank is enamel reactor; Alkene hydrochloric acid in diluted acid reaction tank utilizes acid proof pump to extract from fresh acid storage pond; Inorganic salts is Fe salt, Ca salt, Al salt;
3) by step 2) in solidliquid mixture in plate-and-frame filter press, carry out solid-liquid separation, the liquid separated is spent acid, and spent acid is put into step 1) material stock pond carry out spent acid recycling; Described plate-and-frame filter press adopts acidproof filter cloth;
4) by step 3) in silicon rubber pyrolysis lime-ash after press filtration put into that high-temperature roasting furnace system carries out drying, high-temperature calcination, dust-removal and desulfurizing, simultaneously introducing air, form oxidation atmosphere, oxidation removal organism, obtains white carbon black powder;
5) by step 4) white carbon black powder of gained puts into cooling kiln and carries out cooling down, obtained white carbon black; SiO in described white carbon black
2content is the 91-94% of gross weight, and the 6-9% of residue gross weight is wrapped in not by the inorganic salts of hydrochloric acid stripping in silicon rubber pyrolysis lime-ash particulate, and this part inorganic salts, after high-temperature roasting, solidifies in white carbon black particulate.
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| CN201310077903.5A CN103130230B (en) | 2013-03-12 | 2013-03-12 | Technique for producing white carbon black from silicon rubber pyrolysis ash |
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| CN201310077903.5A CN103130230B (en) | 2013-03-12 | 2013-03-12 | Technique for producing white carbon black from silicon rubber pyrolysis ash |
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| CN103130230A CN103130230A (en) | 2013-06-05 |
| CN103130230B true CN103130230B (en) | 2015-04-22 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2526778B (en) * | 2014-04-17 | 2018-05-30 | Avon Polymer Prod Ltd | Rubber processing method |
| CN111253623B (en) * | 2020-03-24 | 2021-08-03 | 广东省稀有金属研究所 | Method for utilizing waste silicon rubber chlorosilane method cracking slag |
| CN113447393A (en) * | 2020-03-28 | 2021-09-28 | 北京橡院橡胶轮胎检测技术服务有限公司 | Method for quantitatively determining content of silicon dioxide in silicone rubber |
| CN113484209B (en) * | 2021-05-24 | 2023-08-18 | 浦林成山（山东）轮胎有限公司 | Identification method of white carbon black in vulcanized rubber and application thereof |
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| US7892643B2 (en) * | 2004-09-30 | 2011-02-22 | Cabot Corporation | Metal and oxides thereof and methods to make same |
| JP4799265B2 (en) * | 2006-05-17 | 2011-10-26 | 東ソー・クォーツ株式会社 | Surface modification method for silicon dioxide material, surface-modified silicon dioxide material and composite material thereof |
| CN101254922A (en) * | 2008-04-01 | 2008-09-03 | 大连理工大学 | Method for preparing modified white carbon black by using oil shale oil-making residual |
| CN102491348A (en) * | 2011-12-07 | 2012-06-13 | 江山市华顺有机硅有限公司 | Method for preparing white carbon black by utilizing waste silicon rubber cracked residues |
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