CN101823738B - Method for co-production of fine calcium carbonate and sodium silicate, in preparation of light magnesium carbonate by chlor-alkali brine sludge - Google Patents
Method for co-production of fine calcium carbonate and sodium silicate, in preparation of light magnesium carbonate by chlor-alkali brine sludge Download PDFInfo
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- CN101823738B CN101823738B CN2010101696394A CN201010169639A CN101823738B CN 101823738 B CN101823738 B CN 101823738B CN 2010101696394 A CN2010101696394 A CN 2010101696394A CN 201010169639 A CN201010169639 A CN 201010169639A CN 101823738 B CN101823738 B CN 101823738B
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Abstract
The invention discloses a method for co-production of fine calcium carbonate and sodium silicate, in the preparation of light magnesium carbonate by chlor-alkali brine sludge. In the method, brine sludge is filter-washed through a washing filter, and calcium compounds, magnesium compounds, silicon compounds and the like in the brine sludge are then respectively converted into magnesium carbonate, calcium carbonate and sodium silicate in an effective way through carbonation, filtration, centrifugation and the like. Therefore, the method fully develops the potential value of the brine sludge, and provides an economical and effective way for comprehensive utilization of the brine sludge.
Description
Technical field
The present invention relates to the working method of magnesiumcarbonate and lime carbonate, particularly, relate to a kind of method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry.
Background technology
The chlor-alkali salt slurry is from the pulpous state discharge that is produced in the refining crude salt process, and the sedimentary discharge of gained is a sea salt mud behind the salt solution separate part sodium-chlor.The staple of salt slurry is Natural manganese dioxide, quicklime, silicon-dioxide, permanent white and a spot of sodium-chlor and mud.Thereby potential huge utility value.Yet at present, the salt slurry of most of producers is not effectively handled and is utilized, and only is used to build dykes and dams and roadbed material after the dehydration, perhaps in factory, stacks throughout the year.Near perhaps directly entering rivers,lakes and seas, thus cause serious environmental to pollute.
The complicated component that salt slurry contains brings certain difficulty to industrial utilization, but because of its potential utility value, people also constantly explore the salt slurry utilization of waste material, are converted into the method for useful Industrial products.Application number is that 200310122805.5 patent of invention discloses a kind of technology of utilizing the chlor-alkali salt slurry to produce ultra-fine barium sulfate and lime carbonate; Its process characteristic is that the salt material-mud is earlier through strainer filtering; Dry; Calcining obtains ultra-fine barium sulfate through technological processs such as dissolving with hydrochloric acid, separation, washing, drying, comminution by gas stream again; The filtrating of filtering gained adds ammoniacal liquor and transfers pH to remove impurity such as ferrimanganic, and the clear liquid after the removal of impurities adds volatile salt and tensio-active agent, stirs, reaction obtains calcium carbonate superfine powder.The advantage of this invention is utilization of waste material, has reduced environmental pollution, and from salt slurry, produces ultra-fine barium sulfate and the lime carbonate obtain, for the comprehensive utilization of salt slurry provides a new way.Yet this is invented said technology and has only utilized permanent white and the calcium cpd that is contained in the salt slurry, magnesium compound and silicon compound are not utilized and excavation, thereby, be not the technology of the comprehensive utilization of an ideal salt slurry.
Therefore, in order fully to extract and utilize the effective constituent in the salt slurry,, be necessary to carry out new exploration and research for the comprehensive utilization of salt slurry provides cost-effective approach.
Summary of the invention
For this reason; The invention provides a kind of method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry; Compounds such as the calcium that contains in the salt slurry, magnesium, silicon are effectively extracted and utilized to this method; Given full play to the potential value of salt slurry, for the comprehensive utilization of salt slurry provides cost-effective approach.
Technical scheme of the present invention is: a kind of method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry comprises the steps:
A: the chlor-alkali salt slurry with washing filter (1) filter wash three times, is removed the acid group impurity of solubility; At this moment, contain in the salt slurry with Natural manganese dioxide, quicklime and silicon-dioxide are the compound of staple;
B: steps A gained salt slurry is put in first carbonizer (2), and in first carbonizer (2) in according to salt slurry contained Natural manganese dioxide and the mass ratio 1: 1.8～2.2 of carbonic acid gas pure substance feed dioxide gass, carry out carburizing reagent; This moment, Magnesium hydrogen carbonate or magnesiumcarbonate were produced in the reaction of Natural manganese dioxide and carbonic acid gas and water, and the two is water soluble all; Quicklime and carbon dioxide reaction are produced lime carbonate, and lime carbonate is water insoluble basically, thereby precipitates;
C: step B products therefrom is filtered through first filter (4), obtain first filter cake and first settled solution; Be staple with lime carbonate and silicon-dioxide in said first filter cake; Be main with Magnesium hydrogen carbonate or magnesiumcarbonate in first settled solution;
Resulting first settled solution of D: step C obtains light-weight magnesiumcarbonate product (17) through slurry tank (5) thermal degradation, dry, selection by winnowing wrapping machine (7) packing of sedimentation moisture eliminator (6);
E: first filter cake and ammonium chloride that step C obtains are put into reaction in the corrosion-resistant reactor (8) according to the mass ratio 1: 0.87～1.27 of the pure substance of lime carbonate and ammonium chloride; Generate calcium chloride and ammoniacal liquor and dioxide gas; Filter through second strainer (9), get second filter cake and second clear filtrate; Be main with silicon-dioxide in second filter cake, its mass content reaches 80%; Be main with calcium chloride and ammoniacal liquor in second clear filtrate;
F: second clear filtrate that step e obtains is knocked down second carbonizer (10); Using mass concentration is that 1～5% tensio-active agent carries out surface treatment; Stir speed (S.S.) is 120～220r/min, and in second carbonizer (10), feeds dioxide gas, and making calcium chloride and carbonic acid gas in second clear filtrate is 1: 0.19～0.59 to carry out carbonization according to the ratio of the quality of pure substance; Product filters through the 3rd strainer (12), gets the 3rd filter cake of clarifying ammonium chloride filtrating and white; The 3rd filter cake is a lime carbonate;
G: the 3rd filter cake of the white of step e gained is through washing machine (13) washing, moisture eliminator (14) drying, kibbler (15), obtains fine calcium carbonate product (18);
H: resulting second filter cake of step e is put into revolving horizontal drum reactor drum (16) lining with the mass ratio 1: 1.11～1.51 of the pure substance of sodium hydroxide with sodium hydroxide according to silicon-dioxide; Reaction is hydrolyzed; The sodium silicate aqueous solution of reaction solution body is water glass (19).
Measure the carburizing reagent terminal point with the first carbonization table (3) among the step B.
Measure the carburizing reagent terminal point with the second carbonization table (11) in the step F.
Used dioxide gas is pure carbon dioxide gas or carbonic acid gas volume content greater than 20% mixed gas in step B and the step F.
Said tensio-active agent is selected from emulsifiable concentrate, tween 80 and the mixture of the two.
Method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass of the present invention with the chlor-alkali salt slurry, its chemical equation is:
MgO+2CO
2+H
2O＝Mg(HCO
3)
2
MgO+CO
2＝MgCO
3
Mg(HCO
3)
2＝MgCO
3+H
2O+CO
2
CaCO
3+2NH
4Cl+H
2O＝CaCl
2+CO
2+2NH
4OH
CaCl
2+CO
2+2NH
4OH＝CaCO
3+2NH
4Cl+H
2O
SiO
2+2NaOH＝Na
2SiO
3+H
2O
Method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry of the present invention; Effectively extract and utilized compounds such as the calcium that contains in the salt slurry, magnesium, silicon; Given full play to the potential value of salt slurry, for the comprehensive utilization of salt slurry provides cost-effective approach.This method is simple, processing ease, and economic benefit is higher.
Description of drawings
Fig. 1 has showed method technical process of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry of the present invention, wherein,
(1): washing filter (2): first carbonizer (3): the first carbonization table
(4): first strainer (5): slurry tank (6): sedimentation moisture eliminator
(7): selection by winnowing wrapping machine (8): corrosion-resistant reactor (9): second strainer
(10): second carbonizer (11): the second carbonization table (12): the 3rd strainer
(13): washing machine (14): moisture eliminator (15): kibbler
(16): revolving horizontal drum reactor drum (17): magnesiumcarbonate product (18): calcium carbonate product,
(19): water glass
Embodiment
Further describe and explain method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass according to the invention below in conjunction with specific embodiment, disclose materials such as how utilizing method extraction of the present invention and utilize in the salt slurry Natural manganese dioxide that contained, quicklime, silicon-dioxide with the chlor-alkali salt slurry.
Chlor-alkali salt slurry according to the invention is from the salt slurry that obtains for raw material salt manufacturing with sea salt.Through detecting, magnesian mass content is 19.34% in the used salt slurry of following embodiment, and the mass content of quicklime is 19%, and the mass content of silicon-dioxide is 21.88%.
Embodiment one
A kind of method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry; Comprise the steps: 500kg chlor-alkali salt slurry with washing filter (1) filter wash three times; Remove the acid group impurity of solubility; At this moment, contain in the salt slurry with Natural manganese dioxide, quicklime and silicon-dioxide are the compound of staple; Then, the gained salt slurry is put in first carbonizer (2), and in first carbonizer (2), fed pure carbon dioxide gas, make Natural manganese dioxide contained in the salt slurry and carbonic acid gas carry out carbonization at 1: 2.0 according to the mass ratio of pure substance; This moment, Magnesium hydrogen carbonate or magnesiumcarbonate were produced in the reaction of Natural manganese dioxide and carbonic acid gas and water, and the two is water soluble all; Quicklime and carbon dioxide reaction are produced lime carbonate, and lime carbonate is water insoluble basically, thereby precipitates; The carburizing reagent products therefrom being filtered through first filter (4), obtain first filter cake and first settled solution, is staple with lime carbonate and silicon-dioxide in said first filter cake, is main with Magnesium hydrogen carbonate or magnesiumcarbonate in first settled solution; First settled solution obtains fine Magnesium Carbonate Light 41-45 product (17) through slurry tank (5) thermal degradation, dry, selection by winnowing wrapping machine (7) packing of sedimentation moisture eliminator (6); First filter cake and ammonium chloride are put into reaction in the corrosion-resistant reactor (8) according to the mass ratio of the pure substance of lime carbonate and ammonium chloride at 1: 1.27; Generate calcium chloride and ammoniacal liquor and dioxide gas; Filter through second strainer (9), get second filter cake and second clear filtrate; Be main with silicon-dioxide in second filter cake, its mass content reaches 80%; Be main with calcium chloride and ammoniacal liquor in second clear filtrate; Second clear filtrate is knocked down second carbonizer (10); Using mass concentration is that 1% tensio-active agent emulsifiable concentrate is handled; Stir speed (S.S.) is 220r/min; And the carbon dioxide containing gas volume is 25% mixed gas in second carbonizer (10); Making calcium chloride and carbonic acid gas in second clear filtrate is to carry out carbonization at 1: 0.19 according to the ratio of the quality of pure substance, and carbonation reaction temperature is controlled to be 10～20 ℃ of products and filters through the 3rd strainers (12), the 3rd filter cake of clarifying ammonium chloride filtrating and white; The 3rd filter cake is a lime carbonate; The 3rd filter cake of white is through washing machine (13) washing, moisture eliminator (14) drying, kibbler (15), obtains fine calcium carbonate product (18); Second filter cake is put into revolving horizontal drum reactor drum (16) lining with the mass ratio of the pure substance of sodium hydroxide 1: 1.11 with sodium hydroxide according to silicon-dioxide, the reaction that is hydrolyzed, and the sodium silicate aqueous solution of reaction solution body is water glass (19).
Embodiment two
A kind of method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry; Comprise the steps: 500kg chlor-alkali salt slurry with washing filter (1) filter wash three times; Remove the acid group impurity of solubility; At this moment, contain in the salt slurry with Natural manganese dioxide, quicklime and silicon-dioxide are the compound of staple; Then, the gained salt slurry is put in first carbonizer (2), and in first carbonizer (2), to feed the carbon dioxide containing gas volume be 25% mixed gas, make Natural manganese dioxide contained in the salt slurry and carbonic acid gas carry out carbonization at 1: 1.8 according to the mass ratio of pure substance; This moment, Magnesium hydrogen carbonate or magnesiumcarbonate were produced in the reaction of Natural manganese dioxide and carbonic acid gas and water, and the two is water soluble all; Quicklime and carbon dioxide reaction are produced lime carbonate, and lime carbonate is water insoluble basically, thereby precipitates; The carburizing reagent products therefrom being filtered through first filter (4), obtain first filter cake and first settled solution, is staple with lime carbonate and silicon-dioxide in said first filter cake, is main with Magnesium hydrogen carbonate or magnesiumcarbonate in first settled solution; First settled solution obtains Magnesium Carbonate Light 41-45 product (17) through slurry tank (5) thermal degradation, dry, selection by winnowing wrapping machine (7) packing of sedimentation moisture eliminator (6); First filter cake and ammonium chloride are put into reaction in the corrosion-resistant reactor (8) according to the mass ratio of the pure substance of lime carbonate and ammonium chloride at 1: 1.0; Generate calcium chloride and ammoniacal liquor and dioxide gas; Filter through second strainer (9), get second filter cake and second clear filtrate; Be main with silicon-dioxide in second filter cake, its mass content reaches 80%; Be main with calcium chloride and ammoniacal liquor in second clear filtrate; Second clear filtrate is knocked down second carbonizer (10); Using mass concentration is 3% surfactant treatment; Stir speed (S.S.) is 180r/min, and wherein containing mass concentration in the tensio-active agent and be 2% emulsifiable concentrate and mass concentration is 2% tween 80, and the carbon dioxide containing gas volume is 40% mixed gas in second carbonizer (10); Making calcium chloride and carbonic acid gas in second clear filtrate is to carry out carbonization at 1: 0.30 according to the ratio of the quality of pure substance; Carbonation reaction temperature is controlled to be 35～40 ℃, and product filters through the 3rd strainer (12), gets the 3rd filter cake of clarifying ammonium chloride filtrating and white; The 3rd filter cake is a lime carbonate; The 3rd filter cake of white is through washing machine (13) washing, moisture eliminator (14) drying, kibbler (15), obtains fine calcium carbonate product (18); Second filter cake is put into revolving horizontal drum reactor drum (16) lining with the mass ratio of the pure substance of sodium hydroxide 1: 1.35 with sodium hydroxide according to silicon-dioxide, the reaction that is hydrolyzed, and the sodium silicate aqueous solution of reaction solution body is water glass (19).
Embodiment three
A kind of method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry; Comprise the steps: 500kg chlor-alkali salt slurry with washing filter (1) filter wash three times; Remove the acid group impurity of solubility; At this moment, contain in the salt slurry with Natural manganese dioxide, quicklime and silicon-dioxide are the compound of staple; Then, the gained salt slurry is put in first carbonizer (2), and the carbon dioxide containing gas volume is 40% mixed gas in first carbonizer (2), makes Natural manganese dioxide contained in the salt slurry and carbonic acid gas carry out carbonization at 1: 2.2 according to the mass ratio of pure substance; This moment, Magnesium hydrogen carbonate or magnesiumcarbonate were produced in the reaction of Natural manganese dioxide and carbonic acid gas and water, and the two is water soluble all; Quicklime and carbon dioxide reaction are produced lime carbonate, and lime carbonate is water insoluble basically, thereby precipitates; The carburizing reagent products therefrom being filtered through first filter (4), obtain first filter cake and first settled solution, is staple with lime carbonate and silicon-dioxide in said first filter cake, is main with Magnesium hydrogen carbonate or magnesiumcarbonate in first settled solution; First settled solution obtains Magnesium Carbonate Light 41-45 product (17) through slurry tank (5) thermal degradation, dry, selection by winnowing wrapping machine (7) packing of sedimentation moisture eliminator (6); First filter cake and ammonium chloride are put into reaction in the corrosion-resistant reactor (8) according to the mass ratio of the pure substance of lime carbonate and ammonium chloride at 1: 0.87; Generate calcium chloride and ammoniacal liquor and dioxide gas; Filter through second strainer (9), get second filter cake and second clear filtrate; Be main with silicon-dioxide in second filter cake, its mass content reaches 80%; Be main with calcium chloride and ammoniacal liquor in second clear filtrate; Second clear filtrate is knocked down second carbonizer (10); Using mass concentration is that 5% tensio-active agent tween 80 is handled; Stir speed (S.S.) is 120r/min; And in second carbonizer (10), to feed the carbon dioxide containing gas volume be 35% mixed gas; Making calcium chloride and carbonic acid gas in second clear filtrate is to carry out carbonization at 1: 0.59 according to the ratio of the quality of pure substance, and carbonation reaction temperature is controlled to be 10～15 ℃ of products and filters through the 3rd strainers (12), the 3rd filter cake of clarifying ammonium chloride filtrating and white; The 3rd filter cake is a lime carbonate; The 3rd filter cake of white is through washing machine (13) washing, moisture eliminator (14) drying, kibbler (15), obtains fine calcium carbonate product (18); Second filter cake is put into revolving horizontal drum reactor drum (16) lining with the mass ratio of the pure substance of sodium hydroxide 1: 1.51 with sodium hydroxide according to silicon-dioxide, the reaction that is hydrolyzed, and the sodium silicate aqueous solution of reaction solution body is water glass (19).
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting practical range of the present invention, so all equivalences of being done with described characteristic of claim of the present invention and principle change or modify, all should be included within the claim scope of the present invention.
Claims (4)
1. a method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry is characterized in that, comprises the steps:
A: with the chlor-alkali salt slurry with washing filter (1) filter wash three times;
B: steps A gained salt slurry is put in first carbonizer (2), and in first carbonizer (2) in according to salt slurry contained Natural manganese dioxide and the mass ratio 1: 1.8～2.2 of carbonic acid gas pure substance feed dioxide gass, carry out carburizing reagent;
C: step B products therefrom is filtered through first strainer (4), obtain first filter cake and first settled solution;
Resulting first settled solution of D: step C obtains Magnesium Carbonate Light 41-45 product (17) through slurry tank (5) thermal degradation, dry, selection by winnowing wrapping machine (7) packing of sedimentation moisture eliminator (6);
E: first filter cake and ammonium chloride that step C obtains are put into reaction in the corrosion-resistant reactor (8) according to the mass ratio 1: 0.87～1.27 of the pure substance of lime carbonate and ammonium chloride; Generate calcium chloride and ammoniacal liquor and dioxide gas reaction product; Reaction product is filtered through second strainer (9), gets second filter cake and second clear filtrate;
F: second clear filtrate that step e obtains is knocked down second carbonizer (10); Using mass concentration is that 1～5% tensio-active agent carries out surface treatment; Stir speed (S.S.) is 120～220r/min, and in second carbonizer (10), feeds dioxide gas, and making calcium chloride and carbonic acid gas in second clear filtrate is 1: 0.19～0.59 to carry out carbonization according to the ratio of the quality of pure substance; Product filters through the 3rd strainer (12), gets the 3rd filter cake of clarifying ammonium chloride filtrating and white;
G: the 3rd filter cake of the white of step e gained is through washing machine (13) washing, moisture eliminator (14) drying, kibbler (15), obtains fine calcium carbonate product (18);
H: resulting second filter cake of step e is put into revolving horizontal drum reactor drum (16) lining with the mass ratio 1: 1.11～1.51 of the pure substance of sodium hydroxide with sodium hydroxide according to silicon-dioxide; Reaction is hydrolyzed; The sodium silicate aqueous solution of reaction solution body promptly is water glass (19).
2. method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry as claimed in claim 1; It is characterized in that; Measure the carburizing reagent terminal point with the first carbonization table (3) among the step B, measure the carburizing reagent terminal point with the second carbonization table (11) in the step F.
3. method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry as claimed in claim 1; It is characterized in that used dioxide gas is pure carbon dioxide gas or carbonic acid gas volume content greater than 20% mixed gas in step B and the step F.
4. method of producing Magnesium Carbonate Light 41-45 coproduction fine calcium carbonate and water glass with the chlor-alkali salt slurry as claimed in claim 1 is characterized in that said tensio-active agent is selected from emulsifiable concentrate, tween 80 and the mixture of the two.
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| CN2010101696394A CN101823738B (en) | 2010-04-30 | 2010-04-30 | Method for co-production of fine calcium carbonate and sodium silicate, in preparation of light magnesium carbonate by chlor-alkali brine sludge |
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| US9890081B2 (en) | 2015-09-02 | 2018-02-13 | Council Of Scientific & Industrial Research | Functionalized brine sludge material and a process for the preparation thereof |
| US11699533B2 (en) | 2020-10-19 | 2023-07-11 | Council Of Scientific And Industrial Research An Indian Registered Body Incorporated Under The Regn. Of Soc. Act (Act Xxi Of 1860) | Advanced lead-free radiation protection materials utilizing modified brine sludge composition and the process thereof |
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| CN1137488A (en) * | 1995-06-08 | 1996-12-11 | 福建省福州第二化工厂职工技术协会 | Process for preparing magnesium sulfate by using chlorine alkali offscum salt slurry |
| CN1122638C (en) * | 2000-12-06 | 2003-10-01 | 化学工业部连云港设计研究院 | Comprehensive utilization method of waste ammonia sode liquid and sodium sulfate containing waste liquid |
| CN1504412A (en) * | 2002-11-28 | 2004-06-16 | 欣 程 | Method for making superfine calcium carbonate using exhaust gas and liquid from ammonia-soda process for producing sodium carbonate |
| CN1228247C (en) * | 2003-12-25 | 2005-11-23 | 华东理工大学 | Process for producing super fine barium sulfate and calcium carbonate using chloralkali salt mud |
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