CN1321243C - Method for recovering superfine calcium carbonate by clean causticization of green liquor - Google Patents
Method for recovering superfine calcium carbonate by clean causticization of green liquor Download PDFInfo
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- CN1321243C CN1321243C CNB2004100530771A CN200410053077A CN1321243C CN 1321243 C CN1321243 C CN 1321243C CN B2004100530771 A CNB2004100530771 A CN B2004100530771A CN 200410053077 A CN200410053077 A CN 200410053077A CN 1321243 C CN1321243 C CN 1321243C
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Abstract
The present invention relates to a method for recovering superfine calcium carbonate by cleaning and causticizing green liquor. The method mainly comprises the following steps: a. polymeric flocculant is added to green liquor, sediments on the lower layer are removed after the green liquor and the polymeric flocculant are evenly agitated, and clear liquor on the upper layer is retained to be used as refined green liquor for standby; b. quicklime is added to water so as to make calcium hydroxide slurry, and impurities are separated and removed from the calcium hydroxide slurry by a sieve or rotary liquor; c. after the refined green liquor is mixed with the calcium hydroxide slurry, the causticizing reaction is implemented, and a crystal regulating agent is added in the reaction; d. the solid-liquid separation of the causticized slurry is implemented, a filter cake is washed with hot water, and filter liquor is recovered; e. the filter cake is pulped and watered to prepare suspension liquor slurry, and carbon dioxide is introduced so as to obtain superfine calcium carbonate. In the causticizing process, the method is used, the particle sizes are even through the agitation speed rate and the material mixing mode, and thus, the solid-liquid separation effect is enhanced. The recovered superfine calcium carbonate slurry is carbonized secondarily after liquid alkali is filtered, washed and recovered, the product alkalinity is reduced, and the product quality is enhanced.
Description
Technical field:
The black liquor recovery liquid caustic soda that the present invention relates in the papermaking to be produced and the technical field of environmental protection, specifically a kind of green liquor cleaning causticization reclaims the method for calcium carbonate superfine powder.
Background technology:
In the paper mill, when producing, alkaline process system oar produces a large amount of black liquor, serious environment pollution at present.In order to eliminate the pollution of black liquor to environment, each large-scale pulping and paper-making manufacturing enterprise all has black liquor alkali to reclaim, and has eliminated the pollution of black liquor, and the liquid caustic soda of recovery continues on for soda pulping process.The tradition technique for recovering papermaking black liquor alkali is had to a kind of product---and caustic soda (white liquid) produces a large amount of waste residues---white clay simultaneously.In these white claies, both contained the calcium carbonate of causticizing reaction, contain unreacted superfluous lime and raw material (green liquor and lime) again and be entrained to various impurity in the reaction system.This white clay complicated component is a kind of alkaline scrap material of serious environment pollution, and its amount is especially big.Along with the development of paper industry, the especially production-scale expansion of soda pulping process, its pollution is very serious, seriously restricts the sustainable development of national economy.
Years of researches are carried out in domestic processing to soda pulping process recovery white clay that alkali produces, and mainly contain three kinds of processing methods at present: (1) is flashed back into lime with white clay and recycled.Because the white clay silicon content height that straw pulp black liquor produces when reclaiming alkali is being sintered into the accumulation that causes silicon when lime recycles, form the vicious circle that silicon disturbs, influence normally carrying out of alkali recovery.(2) white clay is through PROCESS FOR TREATMENT such as washing, grindings, and the calcium carbonate impurity content that this method reclaims is many, and whiteness has only about 80, can only be as the papermaking filler of low grade.This pearl filler is big to the wearing and tearing of paper machine simultaneously, and the paper mill is not approved, is difficult to apply yet.(3) the white clay waste residue is transported to cement, factory substitutes the part lime stone as the raw material of producing cement, carries out the regeneration of waste material resource.This method is low in economic efficiency, also can't apply.
Up to the present, China existing large-scale soda pulping process factory for reclaiming the white clay that is produced behind the alkali lye, because of there not being good improvement method, can only enter rivers or landfill.In fact this method with the transfer of white clay pollution, is present makeshift just, causes secondary pollution.Chemical system of domestic He'nan University reclaims black liquid alkali and has carried out darker research, and has applied for patent of invention " improved alkali recovering process from paper-making black liquor " (publication number CN1436894A).Because this patent is in the causticization process, the particle size of the calcium carbonate product that reclaims has been done effective control.And be used for papermaking filler and coating as calcium carbonate product, except requirement, the more important thing is requirement to pattern to particle diameter; Secondly, this technology reduces the basicity of calcium carbonate by the secondary causticization.In fact, because causticizing reaction is a reversible reaction, according to the thermodynamic principles of chemical reaction, can not be by increasing the causticizing reaction time and finally reducing the basicity of product fully, so cause the calcium carbonate product alkalinity of recovery higher with the method for washing.
Along with the development of paper-making industry, the calcium carbonate that filler and surface coating are used proposes different particle diameter and pattern requirement.Carry out carbonization generation calcium carbonate in milk of lime, feeding kiln gas, particle size and pattern how to control product have more research, and reclaim liquid caustic soda and calcium carbonate for green liquor causticizing, but never there is the people that particle size control, particle diameter pattern control aspect are studied; When reclaiming calcium carbonate, how effectively the basicity aspect of control recovery product does not have satisfied result yet simultaneously.
Summary of the invention:
The object of the present invention is to provide a kind of improved green liquor cleaning causticization to reclaim the method for calcium carbonate superfine powder, by particle diameter, pattern and the basicity of control recovery calcium carbonate product, making it former cause discarded " white clay " becomes the industrialization product that has than high added value.
To achieve these goals, technical scheme of the present invention is: a kind of green liquor cleaning causticization reclaims the method for calcium carbonate superfine powder, it is characterized in that: the method that described green liquor cleaning causticization reclaims liquid caustic soda and calcium carbonate superfine powder may further comprise the steps: a, to add percentage by weight in green liquor be the high polymer coagulant of 0.01-0.1%, the back natural subsidence stirs, remove lower floor's precipitum, stay supernatant liquid standby as refining green liquor; B, be that the quick lime of 10-25% adds in 40-60 ℃ the hot water and makes calcium hydroxide slurry, above-mentioned slurry is separated removal of impurities with screen cloth or spinning liquid percentage by weight; C, with the above-mentioned refining green liquor that makes with after calcium hydroxide slurry is mixed by 1: 1～1.05 of theoretical reacting dose, in 30-100 ℃, carry out causticizing reaction, and to add in the calcium carbonate quantity percentage by weight be the crystal structure adjusting agent of 0.2-1.5% in reaction; D, the slurry after the causticization is carried out Separation of Solid and Liquid, filter cake is with 50-70 ℃ of hot wash, and filtrate is reclaimed as liquid caustic soda; E, filter cake making beating is added water be mixed with the suspension slurry that solid content is 15-20%, feed the further carbonization of carbon dioxide again and be neutral, obtain the calcium carbonate superfine powder slurry until slurry.
Use the technology used in the present invention be calcium hydroxide slurry with refining after the green liquor causticizing reaction in, according to the basic principle of crystallography, by adding crystal structure adjusting agent, the nucleation of control crystal and the growth rate of each crystal face are to reach particle diameter and pattern is controlled.In the subtractive process of green liquor, remove the colloid material to greatest extent, reduce the viscosity of system, the rate of settling of accelerated particle; In the causticization process, by the hybrid mode of stir speed (S.S.) and material, the nucleation period of control calcium carbonate separated with growth period, and it is even to reach particle size, avoided the existence of fine particle and influenced the rate of settling, the raising solid-liquid separation effect.Calcium carbonate superfine powder slurry to reclaiming carries out the secondary carbonization after filtration again behind the washing and recycling liquid caustic soda, effectively reduce the basicity of product, improves the quality of products.The calcium carbonate superfine powder of the different-shape that is reclaimed by this technology is suitable for different purposes, example is used for papermaking filler for little calcium carbonate that is agglomerated into colored shape, calcium carbonate for grain of rice shape is used for papermaking paint, and can be used as high-grade filling for rubber plastic for ultra-fine granular calcium carbonate through the stearic acid processing.Have good social benefit and considerable economic.
The specific embodiment:
The invention will be further described below in conjunction with embodiment.
The method that green liquor of the present invention cleaning causticization reclaims liquid caustic soda and calcium carbonate superfine powder may further comprise the steps: a, to add percentage by weight in green liquor be the high polymer coagulant of 0.01-0.1%, the back natural subsidence stirs, remove lower floor's precipitum, the viscosity of reduction system, the rate of settling of accelerated particle stays supernatant liquid standby as refining green liquor; B, be that the quick lime of 10-25% adds in 40-60 ℃ the hot water and makes calcium hydroxide slurry with percentage by weight, above-mentioned slurry screen cloth or spinning liquid are separated removal of impurities, calcium hydroxide slurry behind the quicklime slaking being carried out spinning liquid separate the impurity removal and purification processing, is to enter the causticization system for fear of oxious component; C, by the ratio of the theoretical amount of the reaction of the sodium carbonate in calcium hydroxide and the green liquor be 1.05 mix after, in 30-100 ℃, carry out causticizing reaction, in the causticization process, hybrid mode by stir speed (S.S.) and material, the nucleation period of control calcium carbonate separated with growth period, it is even to reach particle size, avoid the existence of fine particle and influenced the rate of settling, improve solid-liquid separation effect, and adding weight of calcium carbonate percentage is the crystal structure adjusting agent of 0.2-1.5% in reaction, the hybrid mode and the stir speed (S.S.) of control green liquor and calcium hydroxide suspension, the growth rate of regulating each crystal face makes the particle diameter of calcium carbonate and pattern controlled; D, the slurry after the causticization is carried out Separation of Solid and Liquid, filter cake is with 50-70 ℃ of hot wash, and filtrate is reclaimed as liquid caustic soda; E, filter cake making beating is added water be mixed with the suspension slurry that solid content is 15-20%, feed the further carbonization of carbon dioxide again and be neutral, effectively reduce the alkali content in the product, help improving the quality of products, obtain the calcium carbonate superfine powder slurry until slurry.Wherein green liquor be black liquor through calcine sode ash, get with water extraction again, it is a prior art, has here just repeated no more.
In refining calcium hydroxide slurry and the reaction of refining green liquor, the solid content of calcium hydroxide slurry is 25-40%; Add crystal structure adjusting agent in carry out at causticizing reaction preceding 0-40 minute, crystal structure adjusting agent is sodium hydrogen phosphate, sodium sulphate, potassium sulfate, borax and sucrose; The carbon dioxide that adds in the suspension slurry comes from kiln gas or paper plant, and its concentration is 20-35%, and temperature is 10-40 ℃; With the surface conditioning agent that accounts for calcium carbonate superfine powder percentage by weight 1.0～3.5% calcium carbonate superfine powder is carried out surface treatment and make super-fine active calcium carbide, described surface conditioning agent is stearic acid, water-soluble titanate coupling agent AT-15, water-soluble KH-550 silane coupler, and the temperature of processing is 45～90 ℃; The temperature of the final dried of super-fine active calcium carbide is 85～110 ℃.
In force, add sodium polyacrylate polymer flocculant or water soluble starch in green liquor, addition is 0.01～0.1% of an amount of liquid, and the back natural subsidence that stirs is removed lower floor's precipitum, and supernatant liquid is standby for refining green liquor; Quick lime is added in 40～60 ℃ the hot water, static 15～20 minutes, stirred again 15 minutes, thick calcium hydroxide slurry is further separated residue through the secondary cyclone hydraulic separators must make with extra care calcium hydroxide slurry.With this calcium hydroxide slurry natural subsidence, supernatant liquor is used for digesting once more, and lower floor's precipitum is that the calcium hydroxide slurry of high solids is standby; Calcium hydroxide slurry is mixed stirring with the green liquor made from extra care, and be warming up to 50～100 ℃ of reactions, when the conversion ratio of causticizing reaction adds crystal structure adjusting agent sodium hydrogen phosphate, sodium sulphate, potassium sulfate, borax and sucrose etc. 0%～30% the time, addition is 0.2%～1.5% of a calcium carbonate quantity, regulates the particle diameter and the pattern of calcium carbonate.
Reaction equation is: Ca (OH) 2+Na2CO3=CaCO3 ↓+2NaOH
Then the slurry after the causticization is carried out centrifugal dehydration treatment after natural subsidence, the filter cake hot wash.Supernatant liquor, the liquid caustic soda of filtrate for reclaiming can be used for paper industry.Cleaning solution is used for the leaching of sode ash, promptly produces green liquor; Filter cake is added water, and to be mixed with solid content be 15%～20% suspension slurry, under agitation feed the further carbonization of kiln gas (pH is 7) to terminal, this calcium carbonate superfine powder slurry promptly directly is sent to paper plant and makes the calcium carbonate superfine powder coating for paper as papermaking filler or after dewatering; The calcium carbonate superfine powder slurry is heated to 45～95 ℃, adds the processing that coats of 0.5～3.5% covering by the weight of calcium carbonate, coating the processing time is 0.5～3.5 hour.Used covering is one or both in stearic acid, water-soluble titanate coupling agent AT-15 and the water-soluble KH-550 silane coupler etc., its preparation method is 5～20% the aqueous solution for covering being mixed with concentration, regulate pH value of aqueous solution 8～13 in 50～80 ℃ of temperature ranges, dissolving is emulsifiable in the water stand-by.Can be used as the functional stuffing of high-grade rubber, plastics and vehicle paint base by the super-fine active calcium carbide of this method processing.
Embodiment 1
Adding solid content in a certain amount of green liquor is the aqueous solution of 3.0% Sodium Polyacrylate flocculant, and addition is 0.01% of a green liquor amount, mixes the back and filters in static 30 minutes, and clear liquid is used for causticizing reaction.
Quick lime joined in 50 ℃ the hot water, static 15 minutes, stirred again 15 minutes, the calcium hydroxide coarse particles, coarse particles is crossed 200 eye mesh screens, removes residue, after the slurry natural subsidence, extracts supernatant liquor, the calcium hydroxide pulpous state thing of lower floor's high solids.Ratio by the theoretical amount of the reaction of the sodium carbonate in calcium hydroxide and the green liquor is 1.05, be mixed in the causticizing reaction still, under agitation be warming up to 90 ℃, react 0.5% crystal structure adjusting agent sodium citrate aqueous solution of adding calcium carbonate theoretical amount after 10 minutes and continued isothermal reaction 1 hour.After question response is intact, filter causticization liquid, reclaim liquid caustic soda with the hot wash filter cake.Filter cake is pulled an oar after adding clear water, is mixed with that to contain be 15% slurry admittedly, feeds kiln gas at normal temperatures again and carries out the secondary carbonization, is reaction end about the pH of suspension value reduces to 7.This product is fusiform microaggregate, and whiteness is greater than 92, and the pH value is 8.2, and settling volume is 3.1, is suitable for as papermaking filler.
Embodiment 2
After green liquor and calcium hydroxide slurry made with extra care, to be warmed up to 70 ℃ after the mixing of two liquid, isothermal reaction 15 minutes, the aqueous solution that adds 1.0% Boratex of calcium carbonate theoretical amount again continues reaction 1 hour, with embodiment 1 filtered and recycled alkali lye, pull an oar after filter cake added clear water, be made into solid content and be 18% slurry, feed kiln gas at normal temperatures again and carry out the secondary carbonization, about the pH value of suspension reduces to 7, be reaction end.This product is a sheet, and average grain diameter is 0.50 micron, and whiteness is greater than 92.This slurries filtration is got the filter cake of high solids, after dispersion treatment, be applicable to and do papermaking paint.
Embodiment 3
After green liquor and calcium hydroxide slurry made with extra care, add the aqueous solution of 1.0% sucrose of calcium carbonate theoretical amount after two liquid are mixed again, be warmed up to 50～70 ℃, isothermal reaction 1 hour.With embodiment 1 filtered and recycled alkali lye, pull an oar after filter cake added clear water, be made into solid content and be 14% slurry, feed kiln gas at normal temperatures again and carry out the secondary carbonization, about reducing to 7, the pH value of suspension is reaction end.2.5% stearic acid covering of calcium carbonate quantity is dissolved in 90 ℃ the hot water, the pH value that adds the alkali regulator solution carries out emulsification treatment to covering about 13.Covering is joined in the calcium carbonate slurry that is warmed up to 80 ℃ then, the constant temperature coating reaction is 1 hour in the time of 80 ℃, with slurry filtered while hot, drying, final baking temperature is not more than 100 ℃ and gets the super-fine active calcium carbide product, the average grain diameter of this product is 0.15 micron, and whiteness is greater than 92, and activation grade is big by 99%, oil factor is 28～35g/100gCaCO3, and does not have agglomeration.Can be used as the functional stuffing that high-grade rubber, plastics are used.
Claims (8)
1. a green liquor cleans the method that causticization reclaims calcium carbonate superfine powder, it is characterized in that, may further comprise the steps: a, to add percentage by weight in green liquor be the high polymer coagulant of 0.01-0.1%, the back natural subsidence stirs, remove lower floor's precipitum, stay clarification night work in upper strata standby for refining green liquor; B, be that the quick lime of 20-25% adds in 40-60 ℃ the hot water and makes calcium hydroxide slurry, above-mentioned slurry is separated removal of impurities with screen cloth or spinning liquid percentage by weight; C, by the ratio of the theoretical amount of the reaction of the sodium carbonate in calcium hydroxide and the green liquor be 1.05 mixes after, in 30-100 ℃, carry out causticizing reaction, and adding weight of calcium carbonate percentage is the crystal structure adjusting agent of 0.2-1.5% in reaction; D, the slurry after the causticization is carried out Separation of Solid and Liquid, filter cake is with 50-70 ℃ of hot wash, and filtrate is reclaimed as liquid caustic soda; E, filter cake making beating is added water be mixed with the suspension slurry that solid content is 15-20%, feed the further carbonization of carbon dioxide again and be neutral, obtain the calcium carbonate superfine powder slurry until slurry.
2, a kind of green liquor cleaning causticization according to claim 1 reclaims the method for calcium carbonate superfine powder, it is characterized in that, in the coating process of calcium carbonate superfine powder slurry, add and account for calcium carbonate superfine powder percentage by weight 0.5～3.5% covering, coating the processing time is 0.5～3.5 hour, make super-fine active calcium carbide, used covering is stearic acid and water-soluble KH-550 silane coupler.
3, a kind of green liquor cleaning causticization according to claim 1 reclaims the method for calcium carbonate superfine powder, it is characterized in that in refining calcium hydroxide slurry and the reaction of refining green liquor, the solid content of calcium hydroxide slurry is 25-40%.
4, a kind of green liquor cleaning causticization according to claim 1 reclaims the method for calcium carbonate superfine powder, it is characterized in that, add crystal structure adjusting agent in carry out at causticizing reaction preceding 0-40 minute, crystal structure adjusting agent is sodium hydrogen phosphate, sodium sulphate, potassium sulfate, borax and sucrose.
5, a kind of green liquor cleaning causticization according to claim 1 reclaims the method for calcium carbonate superfine powder, it is characterized in that the carbon dioxide that adds in the suspension slurry comes from kiln gas or paper plant, and its concentration is 20-35%, and temperature is 10-40 ℃.
6, a kind of green liquor cleaning causticization according to claim 1 reclaims the method for calcium carbonate superfine powder, it is characterized in that, with the surface conditioning agent that accounts for calcium carbonate superfine powder percentage by weight 1.0～3.5% calcium carbonate superfine powder is carried out surface treatment and make super-fine active calcium carbide, described surface conditioning agent is stearic acid and water-soluble KH-550 silane coupler, and the temperature of processing is 45～90 ℃.
7, a kind of green liquor cleaning causticization according to claim 1 reclaims the method for calcium carbonate superfine powder, it is characterized in that high polymer coagulant is Sodium Polyacrylate or water soluble starch.
8, a kind of green liquor cleaning causticization according to claim 1 reclaims the method for calcium carbonate superfine powder, it is characterized in that the final dried temperature of super-fine active calcium carbide is 85～110 ℃.
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| CN100427678C (en) * | 2006-12-26 | 2008-10-22 | 上海东升新材料有限公司 | Purifying treating process of paper making green liquid and application of abtained white mud |
| CN102303885A (en) * | 2011-08-23 | 2012-01-04 | 陕西科技大学 | Method for refining white clay calcium carbonate from green solution produced in alkali recovery from grass pulp |
| CN103180506A (en) * | 2011-09-19 | 2013-06-26 | 北京沃特玛德环境技术股份有限公司 | Method for comprehensively utilizing solid waste during soda recovery in papermaking industry |
| CN102423608A (en) * | 2011-10-28 | 2012-04-25 | 长沙理工大学 | Desulfurizer prepared by causticized white mud and method thereof for flue gas desulphurization |
| CN102553890A (en) * | 2012-01-18 | 2012-07-11 | 牟作峰 | White mud recycling method |
| CN102659161B (en) * | 2012-05-08 | 2013-12-11 | 山东轻工业学院 | Process for preparing white mud calcium carbonate from green liquor recovered from wood pulp sulfate-method pulping alkali |
| CN102730736A (en) * | 2012-06-28 | 2012-10-17 | 陕西科技大学 | Method for preparing granular white mud calcium carbonate by using green liquor from straw pulp base recovery |
| AT514010B1 (en) * | 2013-02-26 | 2015-02-15 | Mondi Ag | Process for causticizing green liquor |
| CN103754918A (en) * | 2013-12-25 | 2014-04-30 | 闫冉冉 | Method for preparing alkali-recovery lime mud free of components with fine particle sizes |
| CN103897434B (en) * | 2014-04-19 | 2016-03-30 | 芮城新泰纳米材料有限公司 | The preparation method that plastic master batch is Nano calcium carbonate dedicated |
| CN104695270B (en) * | 2015-02-14 | 2016-11-30 | 浙江理工大学 | A kind of non-wood pulping alkali collection green liquor low temperature causticization control silicon method |
| CN105839173A (en) * | 2016-03-21 | 2016-08-10 | 中国制浆造纸研究院 | Preparation method of white mud calcium carbonate whisker |
| CN105883879A (en) * | 2016-04-07 | 2016-08-24 | 安徽江东科技粉业有限公司 | Preparation method of nano-coated composite calcium carbonate |
| CN108978310A (en) * | 2018-08-24 | 2018-12-11 | 四川省犍为凤生纸业有限责任公司 | The processing method and application thereof of white clay high-recovery in a kind of paper-making process |
| CN109650433B (en) * | 2019-02-13 | 2019-12-03 | 广东鼎丰纸业有限公司 | The method of slurrying alkali collection green liquor purification manufacture high-purity calcium carbonate |
| CN113105784A (en) * | 2021-05-10 | 2021-07-13 | 华东理工大学 | Method for producing pigment for coating from papermaking white mud |
| CN114380315B (en) * | 2021-09-22 | 2024-01-26 | 湖南新绿方药业有限公司 | Purification method and production equipment of medicinal calcium carbonate |
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Effective date of registration: 20100129 Address after: Room 1107, building 2, 100 Qinzhou Road, Shanghai, zip code: 200235 Co-patentee after: Yanzhou Mingyang Chemical Co., Ltd. Patentee after: Shanghai Dongsheng new materials Co., Ltd. Address before: No. 1002, room 100, Qinzhou Road, Shanghai: 200235 Co-patentee before: Yanzhou Gaoxu Chemical Industry Co., Ltd. Patentee before: Shanghai Dongsheng new materials Co., Ltd. |