CN1830797A - Method and technology of producing precipitated barium sulphate using white carbon black waste liquor - Google Patents
Method and technology of producing precipitated barium sulphate using white carbon black waste liquor Download PDFInfo
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Abstract
A process for preparing precipitated barium sulfate from the white carbon black sewage is based on BaS+Na2SO4-BaSO4 Na2S, includes such steps as regulating pH value, removing impurities, filtering, concentrating, mixing with the impregnating liquid of black powder, displacement reaction, and solid-liquid separation to obtain said product and liquid-stat Na2S.
Description
Technical Field
The invention relates to a production method of precipitated barium sulfate, in particular to a method for producing precipitated barium sulfate by using white carbon black production waste liquid, and also relates to a production process of precipitated barium sulfate, in particular to a process for producing precipitated barium sulfate by using white carbonblack waste liquid.
Background
At present, two technological methods, namely a mirabilite-black ash method (also called a smelting method) or a synthesis method, are mostly adopted for producing precipitated barium sulfate in China. At present, the precipitated barium sulfate is mostly prepared by using mirabilite-black ash method, which uses natural barite ore and mirabilite as raw materials, firstly, the barite is crushed, then mixed with coal powder, calcined and reduced to produce barium sulfide, namely black ash (with BaS content of about 60%), then the black ash is leached and clarified to obtain the barium sulfateBlack ash solution (BaS content is 15-25%), then the black ash solution is placed in a specific reaction container, and is mixed with the dissolved and clarified mirabilite solution (Na)2SO4Content of between 17 and 20 percent) is subjected to a displacement reaction, and the production reaction formula is . And (3) carrying out solid-liquid separation on the synthetic liquid to obtain a solid phase, namely the precipitated barium sulfate, and washing, adjusting, drying, crushing and packaging to obtain a precipitated barium sulfate finished product. The liquid phase is Na2And concentrating and crystallizing the S solution to obtain the industrial sodium sulfide finished product. The method is a main domestic method for producing precipitated barium sulfate, and the whole production process is shown in attached figure 1. Chinese patent No. CN96118396 discloses a production process for preparing precipitated barium sulfate by a smelting method, which comprises the steps of calcining barite ore at 700-800 ℃, removing impurities, and baking the selected barium sulfate water-containing monomer to prepare barium sulfate. Chinese patent with the patent number CNA1015509 also discloses another smelting methodThe process for preparing precipitated barium sulfate uses potassium chloride or sodium chloride as flux. Mixing barite powder and potassium chloride or sodium chloride at a certain ratio, preheating, smelting, removing impurities, water quenching molten liquid obtained by smelting, grinding, leaching with water, filtering, washing, drying, etc. to obtain pasty or powdery precipitated barium sulfate. However, the existing smelting method for preparing precipitated barium sulfate is limited by resources, is only suitable for producing in places with barite ores, and the quality of the produced product is not high.
The other production method of precipitated barium sulfate is to prepare precipitated barium sulfate by a chemical synthesis method, which generally adopts direct synthesis reaction of barium chloride and sulfuric acid to generate barium sulfate and sodium chloride, but the existing production process needs huge equipment, complex process and high investment, 3000T/year barium sulfate needs to be invested by 400-500 ten thousand yuan per year, and the production cost is high and is generally not adopted.
In addition, some methods for refining and crushing barite raw ore to obtain barium sulfate,
on the other hand, when producing series hydrated precipitated silica (common name white carbon black),has a large amount of sodium sulfate (Na)2SO4) Waste liquid is generated, and 12 tons of waste liquid containing sodium sulfate (Na) is discharged for producing 1 ton of white carbon black products2SO4) Nearly 600 Kg. Thus, not only water resource is created and sodium sulfate (Na) is available2SO4) The waste of resources also causes serious environmental pollution to downstream water and land, and brings a series of environmental protection problems. The problem is mainly treated by further diluting with water and then discharging, but the method is not ideal from the practical effect, and the problem is not solved fundamentally even though huge capital is invested for treatment, and larger water resource waste is caused. While sodium sulfate (Na) is simply recovered2SO4) And the concentration is too low, so that the method has no economic value. Therefore, how to economically and circularly utilize the waste liquid becomes an urgent and practical problem of sustainable development of white carbon black production.
Disclosure of Invention
The invention aims to provide a novel precipitated barium sulfate production method and process aiming at the defects of the existing precipitated barium sulfate production process.
The technical implementation proposed according to the object of the invention is: the waste liquid of white carbon black is treated to replace mirabilite in conventional production of precipitated barium sulfate, and the precipitated barium sulfate is prepared by using the waste liquid of white carbon black, namely a black ash method. The black ash method of the white carbon black waste liquid is as follows: the white carbon black waste liquid is subjected to adjustment, impurity removal, filtration and concentration, then is mixed with black ash leaching liquid, and is subjected to displacement reaction and solid-liquid separation to obtain precipitated barium sulfate and industrial liquid sodium sulfide. The production reaction formula is . The specific preparation process comprises the following steps: the barite is first prepared into black ash leaching solution by conventional method, or directly leached, filtered and adjusted with black ash to obtain black ash leaching solution, and the blackash leaching solution is then mixed with bariteThe white carbon black waste liquid is treated, because the main component of the white carbon black waste liquid is sodium sulfate (Na)2SO4) About 8 percent and a small amount of H+、Al3+、Mg2+、Ca2+、SiO2The white carbon black waste liquid is not directly used because of the fine particle impurities, and OH with the concentration of 0.1-1 percent is required to be used firstly-Removing H in the white carbon black waste liquid+(ii) a Then use CO in the impurity removal tank3 2-、OK-、S2-The comprehensive treating agent is used for respectively removing Al according to the concentration of 0.1-1% and different sequences3+、Mg2+、Ca2+Ion and precipitating SiO by flocculating agent2Microparticles; then the pure sodium sulfate (Na) is obtained by precise filtration2SO4) Mother liquor; reconcentrating and evaporating to 17-22% sodium sulfate (Na)2SO4) And (3) solution. After adjustment, impurity removal, filtration and concentration, the white carbon black waste liquid is changed into the white carbon black waste liquid only containing sodium sulfate (Na)2SO4) The solution of (1). Mixing the treated white carbon black waste liquid with the black ash leaching solution, performing a displacement reaction (according to the ratio of the white carbon black waste liquid to the black ash leaching solution of 100: 10-30), and performing solid-liquid separation on the reacted liquid after the displacement reaction, wherein the solid-liquid separation is mainly realized by a filter pressing method. Wherein the liquid phase is industrial liquid sodium sulfide (concentration 25%), composed ofThe liquid separated by the solid-liquid separation device is obtained by evaporation, concentration and crystallization; after solid-liquid separation, the solid phase is precipitated barium sulfate, and the precipitated barium sulfate is washed, dried and crushed to form a common barium sulfate product. The precipitated barium sulfate obtained by filter pressing can also be prepared into a superfine barium sulfate product by modification, filter pressing, drying and crushing. In the process: the drying adopts a flash evaporation drying process and a totally-enclosed circulating airflow drying process; the separation and washing adopts dynamic washing solid-liquid separation equipment, and the washing effect is controlled to the maximum extent by utilizing the solute diffusion homogenization principle with different concentrations; different functional sections are combined and decomposed into modularized thermal sections, so that the difficulties of combustion, radiation, conduction and condensation of each section are avoided.
The invention is characterized in that: sodium sulfate in white carbon black waste liquid in the production of hydrated precipitated silica is fully utilized to replace the original mirabilite solution, and precipitated barium sulfate and industrial liquid sodium sulfide are produced through synthesis and replacement, so that the production cost of barium sulfate is reduced, and the problem of waste liquid pollution in the production of the hydrated precipitated silica is solved. And because of adopting the totally-enclosed circulating airflow drying process, thoroughly eliminating impurity pollution and improving the product quality; the drying adopts a novel flash drying process, so that the drying is not required to be smashed again; by adopting dynamic washing solid-liquid separation equipment and utilizing the solute diffusion homogenization principle with different concentrations, the washing effect can be controlled to the maximum extent, thereby saving water resources, improving the production efficiency and improving the product quality. 5 tons of water are used for producing 1 ton of BaSO4, and 8 tons of water are saved compared with the traditional process; the washing qualification rate reaches 100 percent and is improved by 15 percent compared with the qualification rate of 85 percent of the original washing procedure; the production efficiency is improved by 20 percent compared with the original process; different functional sections are combined and decomposed into modularized thermal sections, so that the difficulties of combustion, radiation, conduction and condensation of the sections are avoided, the thermal sections are decomposed and utilized, and the optimal heat energy utilization rate is achieved. Not only saving the investment 1/4, but also adjusting the heating capacity, improving the comprehensive heat benefit to 88 percent, and improving the comprehensive heat benefit by 38 percent compared with the traditional equipment. A pressure leaching process; the pressure leaching is adopted by utilizing the principle that the pressure is different and the saturated water temperature is different, and the equation P1V1/T1 is P2V 2/T2. The investment is saved by 50 percent compared with the traditional process, the material yield is improved by 5 percent, and the productivity is improved by 100 percent.
Drawings
FIG. 1 is a diagram of a conventional precipitated barium sulfate production process;
FIG. 2 is a diagram of the process for producing precipitated barium sulfate according to the present invention.
Detailed Description
The present invention will be further described with reference to examples.
Example one
The whitecarbon black waste liquid in the production of hydrated precipitated silica is utilized, and the white carbon black waste liquid is subjected to adjustment, impurity removal, filtration and concentration to obtain the white carbon blackThe white carbon black waste liquid is changed to only contain sodium sulfate (Na)2SO4) The solution of (1). The precipitated barium sulfate is prepared by adopting a white carbon black waste liquid-black ash method. The black ash method of the white carbon black waste liquid is as follows: the white carbon black waste liquid is subjected to adjustment, impurity removal, filtration and concentration, then is mixed with the black ash leaching solution, and is subjected to displacement reaction and solid-liquid separation to obtain precipitated barium sulfate and precipitated sodium sulfide. The production reaction formula is . The specific process comprises the following steps:
1. putting the white carbon black waste liquid into an adjusting tank and using OH-(0.1-1% concentration) removal of H+；
2. Then use CO in the impurity removal tank3 2-、OK-、S2-The comprehensive treating agent is used for respectively removing Al according to the concentration of 0.1-1% and different sequences3+、Mg2+、Ca2+Ion and precipitating SiO by flocculating agent2Microparticles;
3. then the pure sodium sulfate (Na) is obtained by precise filtration2SO4) Mother liquor;
4. reconcentrating and evaporating to 17-22% sodium sulfate (Na)2SO4) A solution;
5. leaching and clarifying black ash to obtain black ash leaching solution;
6. mixing the treated white carbon black waste liquid and the black ash leaching solution according to the proportion of 100: 10, and sending the mixture into a displacement tank for displacement reaction;
7. and (3) carrying out solid-liquid separation on the liquid after the replacement reaction, wherein the solid-liquid separation is mainly carried out by a filter pressing method. Wherein the liquid phase is industrial liquid sodium sulfide (concentration is 25%), and the liquid separated by the solid-liquid separation device is obtained by evaporation concentration and crystallization; after solid-liquid separation, the solid phase is precipitated barium sulfate, and the precipitated barium sulfate is washed, dried and crushed to form a common barium sulfate product. Wherein, the drying adopts a flash evaporation drying process and a totally-enclosed circulating airflow drying process; the separation and washing adopts dynamic washing solid-liquid separation equipment, and the washing effect is controlled to the maximum extent by utilizing the solute diffusion homogenization principle with different concentrations; different functional sections are combined and decomposed into modularized thermal sections, so that the difficulties of combustion, radiation, conduction and condensation of each section are avoided.
Example two
The white carbon black waste liquid in the production of hydrated precipitated silica is adjusted, purified, filtered and concentrated to change the white carbon black waste liquid into the white carbon black waste liquid only containing sodium sulfate (Na)2SO4) The solution of (1). The precipitated barium sulfate is prepared by adopting a white carbon black waste liquid-black ash method. The black ash method of the white carbon black waste liquid is as follows: the white carbon black waste liquid is subjected to adjustment, impurity removal, filtration and concentration, thenis mixed with the black ash leaching solution, and is subjected to displacement reaction and solid-liquid separation to obtain precipitated barium sulfate and precipitated sodium sulfide. The production reaction formula is . The specific process comprises the following steps:
1. preparing black ash immersion liquid from barite by a conventional method;
2. putting the white carbon black waste liquid into an adjusting tank and using OH-(0.1-1% concentration) removal of H+；
3. Then use CO in the impurity removal tank3 2-、OK-、S2-The comprehensive treating agent is used for respectively removing Al according to the concentration of 0.1-1% and different sequences3+、Mg2+、Ca2+Ion and precipitating SiO by flocculating agent2Microparticles;
4. then the pure sodium sulfate (Na) is obtained by precise filtration2SO4) Mother liquor;
5. reconcentrating and evaporating to 17-22% sodium sulfate (Na)2SO4) A solution;
6. mixing the treated white carbon black waste liquid and the black ash leaching solution according to the proportion of 100: 10, and sending the mixture into a displacement tank for displacement reaction;
7. and (3) carrying out solid-liquid separation on the liquid after the replacement reaction, wherein the solid-liquid separation is mainly carried out by a filter pressing method. Wherein the liquid phase is industrial liquid sodium sulfide (concentration is 25%), and the liquid separated by the solid-liquid separation device is obtained by evaporation concentration and crystallization; after solid-liquid separation, the solid phase is precipitated barium sulfate, and then the superfine barium sulfate product is prepared by modification, filter pressing, drying and crushing. Wherein, the drying adopts a flash evaporation drying process and a totally-enclosed circulating airflow drying process; the separation and washing adopts dynamic washing solid-liquid separation equipment, and the washing effect is controlled to the maximum extent by utilizing the solute diffusion homogenization principle with different concentrations; different functional sections are combined and decomposed into modularized thermal sections, so that the difficulties of combustion, radiation, conduction and condensation of each section are avoided.
Claims (7)
1. The method and the process for producing the precipitated barium sulfate by using the white carbon black waste liquid are characterized in that: the method comprises the following steps of (1) treating the waste liquid of white carbon black by using the waste liquid in the production of white carbon black, replacing mirabilite in the production of conventional precipitated barium sulfate, and preparing precipitated barium sulfate by using the waste liquid of white carbon black-black ash method, wherein the waste liquid of white carbon black-black ash method comprises the following steps: the white carbon black waste liquid is subjected to adjustment, impurity removal, filtration and concentration, then is mixed with black ash leaching liquid, and is subjected to displacement reaction and solid-liquid separation to obtain precipitated barium sulfate and industrial liquid sodium sulfide.
2. The method and process for producing precipitated barium sulfate as claimed in claim 1, wherein: the preparation process of the white carbon black waste liquid-black ash method comprises the following steps:firstly, preparing black ash leaching liquid from barite by conventional method, and simultaneously placing white carbon black waste liquid in a regulating tank with 0.1-1% OH-Removing H in the white carbon black waste liquid+(ii) a Reuse of CO3 2-、OK-、S2-The comprehensive treating agent is used for respectively removing Al in the white carbon black waste liquid according to the concentration of 0.1-1% and different sequences3+、Mg2+、Ca2+Ion and precipitating SiO by flocculating agent2Microparticles; then pure sodium sulfate mother liquor is obtained through precise filtration; concentrating and evaporating to obtain 17-22% sodium sulfate solution; mixing the treated white carbon black waste liquid with the black ash leaching solution and carrying out displacement reaction; after the displacement reaction, the liquid after the reaction is subjected to solid-liquid separation, and then precipitated barium sulfate and industrial liquid sodium sulfide are obtained according to a conventional process method.
3. The method and process for producing precipitated barium sulfate according to claim 1 or 2, wherein: the black ash leaching solution is obtained by directly leaching, filtering and adjusting black ash.
4. The method and process for producing precipitated barium sulfate according to claim 1 or 2, wherein: the solid-liquid separation is mainly a filter pressing method.
5. The method and process for producing precipitated barium sulfate according to claim 1 or 2, wherein: the liquid phase industrial liquid sodium sulfide is obtained by evaporating, concentrating and crystallizing liquid separated by a solid-liquid separation device.
6. The method and process for producing precipitated barium sulfate according to claim 1 or 2, wherein: the precipitated barium sulfate in the solid-liquid separation solid phase is washed, dried and crushed to form a common barium sulfate product.
7. The method and process for producing precipitated barium sulfate according to claim 1 or 2, wherein: the precipitated barium sulfate in solid-liquid separation solid phase is prepared into a superfine barium sulfate product through modification, filter pressing, drying and crushing after washing, drying and crushing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326499A (en) * | 2014-10-13 | 2015-02-04 | 南风化工集团股份有限公司 | Method for improving sodium sulfide solution concentration by leaching black ash for three times |
| CN106976900A (en) * | 2017-04-14 | 2017-07-25 | 河北科技大学 | A kind of preparation method of powdery paints barium sulfate |
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| JPH075304B2 (en) * | 1989-08-31 | 1995-01-25 | 堺化学工業株式会社 | Barium Sulfate Particle Size Control Method |
| JP3088715B1 (en) * | 1999-04-07 | 2000-09-18 | 鈴茂器工株式会社 | Obi type sushi ball molding machine |
| CN1398789A (en) * | 2002-08-13 | 2003-02-26 | 华北工学院 | Prepn of nano barium sulfate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326499A (en) * | 2014-10-13 | 2015-02-04 | 南风化工集团股份有限公司 | Method for improving sodium sulfide solution concentration by leaching black ash for three times |
| CN104326499B (en) * | 2014-10-13 | 2016-04-27 | 南风化工集团股份有限公司 | By the method for three molten leaching grey black raising sodium sulfide solution concentration |
| CN106976900A (en) * | 2017-04-14 | 2017-07-25 | 河北科技大学 | A kind of preparation method of powdery paints barium sulfate |
| CN106976900B (en) * | 2017-04-14 | 2019-04-05 | 河北科技大学 | A kind of preparation method of powdery paints barium sulfate |
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