CN103086385A - Method for preparing rubber-grade white carbon black by using fly ash - Google Patents
Method for preparing rubber-grade white carbon black by using fly ash Download PDFInfo
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- CN103086385A CN103086385A CN2013100628887A CN201310062888A CN103086385A CN 103086385 A CN103086385 A CN 103086385A CN 2013100628887 A CN2013100628887 A CN 2013100628887A CN 201310062888 A CN201310062888 A CN 201310062888A CN 103086385 A CN103086385 A CN 103086385A
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- carbon black
- sodium
- white carbon
- grade white
- sodium silicate
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Abstract
The invention provides a method for preparing rubber-grade white carbon black by using fly ash, which comprises the following steps that: a sodium silicate solution subjected to solid-liquid separation is injected into an exchanger filled with a cation exchange resin, so that sodium ions in the solution are replaced with hydrogen ions in the exchange resin, thereby reducing the sodium ion content; and the obtained sodium silicate solution with an extremely high silicon-sodium ratio flows out of the lower part of the exchanger and then is subjected to direct carbon separation, thereby obtaining the rubber-grade white carbon black. The exchange resin reaches a saturated state after a period of time, and can be subjected to regeneration treatment and recycling by using a hydrochloric acid solution with a certain concentration, and then a sodium chloride solution generated in the process of resin regeneration treatment can be reused as an industrial salt. A rubber-grade white carbon black product prepared by using the method provided by the invention is stable, the original technological process is simplified, and the added value of products is increased.
Description
Technical field
The present invention relates to the Ash Utilization utilization, specifically belong to a kind of method by the standby rubber grade white carbon black of coal ash for manufacturing.
Background technology
During Ash Utilization utilizes, due to the element silicon major part in flyash be present in flyash mullite mutually in, only have a small amount of silicon to be present in glassy phase, comparatively speaking, element silicon in glassy phase can generate sodium silicate solution with the soda lye reaction under low the requirement, and then reaches the purpose of carrying silicon.
At present, to prepare the technical process of rubber grade white carbon black be first flyash and caustic soda to be reacted the generation water glass to middle coal Pingshou group company treated coal ash; The sodium silicate solution salinity that obtains is high, can not directly carry out carbon and divide preparation rubber grade white carbon black, and carbon divides to need to carry out this part sodium silicate solution for the first time; Carbon divides the gained filter cake to dissolve in the remainder sodium silicate solution, increases dioxide-containing silica, and then improves the solution silicon sodium ratio; Carbon divides again, through solid-liquid separation, washing; Drying obtains the rubber grade white carbon black.Whole technical process is more loaded down with trivial details, and energy consumption is large.
Summary of the invention
The objective of the invention is to prepare for the prior art treated coal ash problem that rubber grade white carbon black technique flow process is more loaded down with trivial details, energy consumption is large, a kind of method by the standby rubber grade white carbon black of coal ash for manufacturing is provided, this method technique is simple, energy consumption is low.
Present method is to utilize to contain sulfonic group (-SO
3H) storng-acid cation exchange resin is met hydrogen ion that solution discharges and the sodium ion generation replacement(metathesis)reaction in solution out, and specifically reaction equation is:
Na
++—SO
3H→—SO
3Na+H
+
It is to utilize certain density hydrochloric acid to carry out backwash to the state resin that reaches capacity that resin regeneration is processed, and concrete reaction equation is:
—SO
3Na+HCl→NaCl+—SO
3H
A kind of method by the standby rubber grade white carbon black of coal ash for manufacturing provided by the invention, concrete steps comprise:
1) by massfraction, first add water at the bottom of 300-500 part in reactor with pressure, add again 200-400 part aluminous fly-ash to dissolve, and the unlatching heating unit, when temperature reaches at 80 ℃, slowly add the sodium hydroxide sheet alkali reaction 20-50min of 98 ﹪ of 50-150 part in the reactor, when temperature reaches 100 ℃-150 ℃, add the water of 600-800 part to dilute in reactor again, after 20min, the solution in reactor is carried out solid-liquid separation, the filtrate that obtains is sodium silicate solution;
2) utilize surge pump, above-mentioned sodium silicate solution is flow through the exchange column that storng-acid cation exchange resin is housed, obtain the high sodium silicate solution of silicon sodium ratio; Described Zeo-karb is strongly acidic styrene type cation exchange resin.
3) under normal temperature and pressure conditions, with the concentration carbon dioxide that is 30 ﹪-35 ﹪ pass into after ion exchange treatment sodium silicate solution in, the flow of carbon dioxide gas amount is controlled at 20m
3/ h, and proportion is that the slow-revving stirrer of the high shear force of 35Hz disperses carbon dioxide, carries out carbon and divides reaction, then carries out solid-liquid separation, washing, drying obtains the rubber grade white carbon black.
Resin is through after a while use, the Na that displaces
+Amount can reach capacity, and exchange capacity reduces, and at this moment should utilize certain density hydrochloric acid soln to carry out backwash and regeneration processing and reuse to the exchange resin of the state of reaching capacity, and the sodium-chlor that manipulation of regeneration produces can prepare Industrial Salt.
Compared with prior art, advantage of the present invention and effect are:
1, method of the present invention can be simplified technique greatly, increases the operability of technique.According to the original mode of production, in the sodium silicate solution of preparing, the concentration of sodium oxide approximately remains on the 50g/L left and right, and the concentration of silicon-dioxide only remains on the 30g/L left and right, and in solution, sodium oxide is dense, the concentration of silicon-dioxide is very low, causes that in sodium silicate solution, salinity is high, silicon sodium ratio is low.In the present invention, utilize storng-acid cation exchange resin that the sodium ion in sodium silicate solution is displaced, reduce the concentration of sodium oxide, make the concentration of sodium oxide be controlled at the 15g/L left and right, improved silicon sodium ratio in solution, and then realize that direct carbon divides the purpose for preparing white carbon black, compare operation with original technique and greatly simplify, and exchange resin used can also reduce production costs in regeneration.The sodium-chlor that manipulation of regeneration produces can prepare Industrial Salt.
2, reduce energy consumption.Use method of the present invention, can make treated sodium silicate solution carry out direct carbon divides and prepares the rubber grade white carbon black, reduced the operation that original technique also needs secondary carbon to divide, both reduced the consumption of carbon dioxide, reduced again secondary carbon and divided required equipment and power consumption etc.
3, improve output.Use method of the present invention, calculate according to processing the 640L sodium silicate solution, the sodium silicate solution after utilization is processed carries out carbon and divides, and can obtain rubber grade white carbon black product 15Kg, compares with original process, and output is improved.
Description of drawings
The standby rubber grade white carbon black technique schema of Fig. 1 coal ash for manufacturing
Embodiment
By reference to the accompanying drawings 1 and embodiment, the present invention is made illustrate.
Embodiment 1
Water first add 400L in reactor with pressure at the bottom of, the 300KG aluminous fly-ash dissolves, and unlatching heating unit, when temperature reached at 80 ℃, slowly adding the 100KG massfraction in the reactor was that the sodium hydroxide sheet alkali of 98 ﹪ reacts 30min, when temperature reaches 100 ℃-150 ℃, add 700L water to dilute in reactor again, after 20min, solution in reactor is sent into fine filting machine and carry out solid-liquid separation, the filtrate that obtains is sodium silicate solution, and in solution, sodium oxide concentration is 50g/L.
Then with surge pump, the sodium silicate solution that obtains is squeezed in the interchanger that strong-acid ion exchange resin is housed that (storng-acid cation exchange resin adopts domestic 001*7 type strongly acidic styrene type cation exchange resin, and the functional group of being with is sulfonic group (-SO
3H).Ion-exchange unit adopts ZFNQ-8 series auto-controlled continuous Na-ion exchanger, belong to automatic control single valve twin columns and produce continuously water floating bed type, twin columns resin filling amount is respectively 410kg, 540kg), keeping solution flow rate is that 6m/h is in interchanger, treatment capacity is 2600L, and the solution oxide na concn is in the 15g/L left and right after plastic resin treatment.
Under normal temperature and pressure conditions, with the concentration carbon dioxide that is 30 ﹪-35 ﹪ pass into after ion exchange treatment sodium silicate solution in, the flow of carbon dioxide gas amount is controlled at 20m
3/ h, and proportion is that the slow-revving stirrer of the high shear force of 35Hz disperses carbon dioxide, carries out carbon and divides reaction, then carries out solid-liquid separation, washing, drying obtains the rubber grade white carbon black.
Pour massfraction from ion-exchanger bottom and be 5% hydrochloric acid soln and resin is carried out backwash and regeneration process, the maintenance flow velocity is 8m/h, keeps 0.5h.Resin can produce electronegative-SO
3 -With positively charged sodium ion Na
+, with the H in hydrochloric acid soln
+And Cl
-Combination respectively, regeneration formation-SO
3The H function group enters next exchange cycle.Solution after manipulation of regeneration can be used to prepare Industrial Salt, increases added value of product.
It is 0.9m that the carbon that we use at present divides the equipment volume of reaction
3, can produce foam during due to aeration-agitation, so add the amount of solution to be strict controlled in 700L, pass at normal temperatures and pressures carbon dioxide, flow control is at 20m
3/ h, carbonic acid gas is when this flow velocity, and utilization ratio is the highest, and carbon divides effect best, flow＜20m
3During/h, carbon divides not exclusively; Flow＞20m
3During/h, can cause carbon dioxide all not dissolve and waste.
Claims (2)
1. the method by the standby rubber grade white carbon black of coal ash for manufacturing, is characterized in that, comprises the following steps:
1) by massfraction, first add water at the bottom of 300-500 part in reactor with pressure, add again 200-400 part aluminous fly-ash to dissolve, and the unlatching heating unit, when temperature reaches at 80 ℃, slowly add the sodium hydroxide sheet alkali reaction 20-50min of 98 ﹪ of 50-150 part in the reactor, when temperature reaches 100 ℃-150 ℃, add the water of 600-800 part to dilute in reactor again, after 20min, the solution in reactor is carried out solid-liquid separation, the filtrate that obtains is sodium silicate solution;
2) utilize surge pump, above-mentioned sodium silicate solution is flow through the exchange column that storng-acid cation exchange resin is housed, obtain the high sodium silicate solution of silicon sodium ratio;
3) under normal temperature and pressure conditions, with the concentration carbon dioxide that is 30 ﹪-35 ﹪ pass into after ion exchange treatment sodium silicate solution in, the flow of carbon dioxide gas amount is controlled at 20m
3/ h, and proportion is that the slow-revving stirrer of the high shear force of 35Hz disperses carbon dioxide, carries out carbon and divides reaction, then carries out solid-liquid separation, washing, drying obtains the rubber grade white carbon black.
2. a kind of method by the standby rubber grade white carbon black of coal ash for manufacturing as claimed in claim 1, is characterized in that step 2) described in storng-acid cation exchange resin be strongly acidic styrene type cation exchange resin.
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| CN2013100628887A CN103086385A (en) | 2013-02-27 | 2013-02-27 | Method for preparing rubber-grade white carbon black by using fly ash |
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|---|---|---|---|
| CN2013100628887A CN103086385A (en) | 2013-02-27 | 2013-02-27 | Method for preparing rubber-grade white carbon black by using fly ash |
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ID=48199590
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110371986A (en) * | 2018-04-13 | 2019-10-25 | 国家能源投资集团有限责任公司 | Carbon divides the processing method of reactor and carbon point method and flyash |
| CN116656140A (en) * | 2023-06-06 | 2023-08-29 | 辽宁兴胜防水材料科技发展有限公司 | Weather-proof polymer modified asphalt waterproof coiled material and production device thereof |
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2013
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110371986A (en) * | 2018-04-13 | 2019-10-25 | 国家能源投资集团有限责任公司 | Carbon divides the processing method of reactor and carbon point method and flyash |
| CN110371986B (en) * | 2018-04-13 | 2021-09-03 | 国家能源投资集团有限责任公司 | Carbon separation reactor, carbon separation method and treatment method of fly ash |
| CN116656140A (en) * | 2023-06-06 | 2023-08-29 | 辽宁兴胜防水材料科技发展有限公司 | Weather-proof polymer modified asphalt waterproof coiled material and production device thereof |
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Application publication date: 20130508 |