CN101838005B - Method for producing sodium chloride and carbon powder and co-producing superfine light calcium carbonate and white carbon black - Google Patents
Method for producing sodium chloride and carbon powder and co-producing superfine light calcium carbonate and white carbon black Download PDFInfo
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Abstract
The invention discloses a method for producing sodium chloride and carbon powder and co-producing superfine light calcium carbonate and white carbon black. Unified alkali waste liquid and carbide slag are used as raw materials, and the method comprises the following steps of: reacting ammonium chloride in the unified alkali waste liquid and calcium hydroxide in the carbide slag to generate carbon filter cake, calcium chloride and ammonium hydroxide, feeding the calcium chloride and the ammonium hydroxide into a carbonation tower and introducing carbon dioxide gas into the carbonation tower to perform carbonation reaction so as to generate calcium carbonate sediment and ammonium chloride solution, and reacting the ammonium chloride solution and water glass to obtain the white carbon black and the sodium chloride. The method for producing the sodium chloride and the carbon powder and co-producing the calcium carbonate and the white carbon black through industrial wastes comprising the unified alkali waste liquid and the carbide slag makes full use of effective ingredients in the industrial wastes, reduces the production cost of industrial products, has simple production process and extremely low production cost, and is a quite economic and effective method.
Description
Technical field
The present invention relates to three industrial wastes comprehensive utilization and process field, particularly, relate to a kind of method of producing fine precipitated calcium carbonate and white carbon black coproduction sodium chloride and carbon dust, the used starting material of this method are waste associated alkali solution and carbide slag.
Background technology
Uniting system soda ash method (be called for short and join alkaline process) is the main method of producing soda ash, is accompanied by the generation of soda ash, also produces a large amount of ammonium chloride exhausted liquids.Can be used for producing nitrogenous fertilizer behind the ammonium chloride exhausted liquid purifying.
Carbide slag is that the resistates that acetylene produced is produced in the calcium carbide hydrolysis; Be the emulsion of solid content at 8%-10%, have another name called calcium carbide mud, its main chemical compositions is a calcium hydroxide; Also contain the aqueous solution such as solid impurities such as Calucium Silicate powder, calcium aluminate, ferrosilicon and breeze and sulfurated lime, calcium hydroxide, acetylene; Being a kind of strong basicity that is, being rich in abundant calcium resource, is that can to produce a series of needs such as lime carbonate, cement calcareous be the product of raw material to raw material with it.But because wherein impurities is more, water cut is high, composition is complicated, undressed carbide slag can't directly utilize.On the other hand; Flourish along with the calcium carbide industry, the quantity discharged of carbide slag also increases day by day, and factory's discharging calcium carbide mud of year producing 200,000 tons of PVC reaches 3,600,000 tons/year; A large amount of carbide slags can't effectively utilize; Directly pile up, cause the soil artificially to alkalize, ecotope is caused the pollution that is difficult to recover severe contamination farmland and underground water.
Preparation WHITE CARBON BLACK (SiO
2) traditional method be the precipitator method: promptly use water glass (water glass) and strong acid, example hydrochloric acid and sulfuric acid, reaction generates the hydrated SiO 2 deposition, is example with hydrochloric acid, its reactive chemistry equation is:
Na
2O·nSiO
2+2HCl+(n·m-1)H
2O→2NaCl+n(SiO
2·mH
2O)↓
Hydrated SiO 2 precipitates the WHITE CARBON BLACK of treated system.This method is produced 1 ton of WHITE CARBON BLACK will consume 4～4.5 tons of water glass and 1.5 tons of hydrochloric acid, and industrial chemicals consumption is big, and is uneconomical.
In order to overcome the defective of traditional method; People have also explored other and have prepared the method for WHITE CARBON BLACK; Like application number is that to disclose a kind of be the method that main raw material prepares WHITE CARBON BLACK with silicofluoric acid, water glass for 200710055061.8 patent of invention; Lower and the raw material of silicofluoric acid cost is easy to get in this method, thereby has reduced the production cost of WHITE CARBON BLACK to a certain extent.Yet this method production technique is very loaded down with trivial details, has especially produced a large amount of by product Sodium Fluorides, and Sodium Fluoride can corrode skin, and stimulating mucosal has disoperation to neural system, thereby having relatively high expectations to production environment and equipment.
Application number is that 200810107069.9 patent of invention discloses a kind of method with producing nano-scale white carbon black with rice hull ash.This method with after the concentrating of the alkaline process Processing of Preparation water glass of rice hull ash, water glass solution again with sulfuric acid reaction, thereby make WHITE CARBON BLACK.This method is not broken away from the defective for preparing WHITE CARBON BLACK with traditional method.Thereby, also be a uneconomic method.
On the other hand, WHITE CARBON BLACK mainly is used as tree elastomer and elastomeric strengthening agent, toothpaste abrasives, also as coating and unsaturated polyester thickening material, and Coating Matting agent, thickening material, plastic film open agent etc.In recent years, along with the fast development of China's process of industrialization, dialogue sooty increasing demand increases, and this has also stimulated the production of WHITE CARBON BLACK greatly, and the price of WHITE CARBON BLACK also constantly raises at present, yet domestic output but can not satisfy the demand in market.
Thereby, ammonium chloride in the development and use waste associated alkali solution and the calcium hydroxide in the carbide slag, it will be a cost-effective method of ten minutes that production simultaneously has the WHITE CARBON BLACK of commercial value and lime carbonate.
Summary of the invention
In order to address the above problem, the invention provides a kind of method of producing superfine light calcium carbonate and white carbon black coproduction sodium chloride and carbon dust, the used starting material of this method are waste associated alkali solution and carbide slag.
Technical scheme of the present invention is: a kind of method of producing superfine light calcium carbonate and white carbon black coproduction sodium chloride and carbon dust, the used starting material of this method are waste associated alkali solution and carbide slag, comprise the steps:
A: convert the mass content of the ammonium chloride in the waste associated alkali solution and the mass content of the calcium hydroxide in the carbide slag respectively;
B: is 1: 1.08～1.45 to drop in the corrosion-resistant reactors (1) carbide slag and waste associated alkali solution according to the pure substance mass ratio of calcium hydroxide and ammonium chloride, reacts, and obtains containing the mixed solution of calcium chloride and ammoniacal liquor;
C: with mixed solution warp first suction filter pump (2) suction filtration that contains calcium chloride and ammoniacal liquor of step B gained, first whizzer (3) is centrifugal, obtains black carbon filter cake and clarifying filtrating;
D: the clarifying filtrating of step C gained is dropped in the carbonating tower (4); Using mass concentration is that 5～10% tensio-active agents carry out surface treatment; Stir speed (S.S.) is 220～320r/min, then feeds dioxide gas and carries out carburizing reagent, obtains carbonated calcium deposit and ammonium chloride mixt;
E: the carbonated calcium deposit and the ammonium chloride mixt of step D gained is centrifugal with second suction filter pump (6) and second whizzer (7), obtain calcium carbonate filter cake and the solution that contains ammonium chloride;
F: with the calcium carbonate filter cake of step e gained successively through washing whizzer (8) washing dehydration, first drying machine (9) drying, kibbler (10) is pulverized, and is packaged to be calcium carbonate product (11);
G: is in 1: 0.64～2.39 input reactor drums (17) with the solution that contains ammonium chloride and the water glass of step e gained according to ammonium chloride and water glass pure substance mass ratio; Under the stirring that blows slowly, carry out two hydrolysis reaction, ammonium chloride is hydrolyzed to ammonia radical ion and cl ions in the aqueous solution, and water glass is hydrolyzed to silicate ion, sodium ion and hydroxide ion in the aqueous solution; The hydrolysis of ammonia radical ion and silicate ion is mutually promoted; Thereby generate ammonia, hydrogen ion and precipitation of silica, hydrogen ion and hydroxide ion directly are combined into water molecules, and precipitation of silica is a WHITE CARBON BLACK; Ammonia effusion solution, cl ions and sodium ion combine to form sodium-chlor;
H: the reaction product of step G gained is filtered through strainer (18), obtain the solution of WHITE CARBON BLACK bullion and sodium chloride-containing;
I: the WHITE CARBON BLACK bullion of step H gained obtains WHITE CARBON BLACK product (20) through second moisture eliminator (19) drying;
J: the solution of the sodium chloride-containing of step H gained is sent into to distill in the underpressure distillation device (21) and is obtained sodium-chlor product (22);
K: said carbon filter cake and excessive hydrochloric acid be excessive response in carbon dust cleaner (12), removes the carbide slag that does not have complete reaction, obtains purified carbon filter cake through the 3rd suction filter pump (13) suction filtration;
L: said purified carbon filter cake through dehydration, dry in carbon dust loft drier (14), is crushed into carbon dust product (16) again in the carbon dust kibbler (15).
With the carbonization terminal point of the said carburizing reagent of chlorination table (5) control, be the carbonization terminal point when reading is motionless to be zero when showing to go up.
The described dioxide gas of step D is pure carbon dioxide gas or carbonic acid gas volume content greater than 20% mixed gas.
Said tensio-active agent is selected from emulsifiable concentrate, tween 80 and the mixture of the two.
Said ammonia returns the utilization of system alkali systemic circulation.
The chemical principle that aforesaid method relates to is:
2NH
4Cl+Ca(OH)
2＝＝＝＝CaCl
2+2NH
4OH
CaCl
2+2NH
4OH+CO
2＝＝＝＝CaCO
3+2NH
4Cl+H2O
2NH
4Cl+Na
2O·nSiO
2＝＝＝＝nSiO
2+2NaCl+2NH
3+H
2O
The method of production superfine light calcium carbonate of the present invention and white carbon black coproduction sodium chloride and carbon dust; Utilize industrial waste product waste associated alkali solution and carbide slag to produce lime carbonate and white carbon black coproduction sodium chloride and carbon dust; Made full use of the effective constituent in the industrial waste product, reduced the production cost of Industrial products, its production process is simple; Production cost is extremely low, is a cost-effective method of ten minutes.
Description of drawings
Fig. 1 has showed the process step of the method for production superfine light calcium carbonate according to the invention and white carbon black coproduction sodium chloride and carbon dust, wherein:
(1)---corrosion-resistant reactor, (2)---first suction filter pump, (3)---first whizzer,
(4)---carbonating tower, (5)---chlorination table, (6)---second suction filter pump,
(7)---second whizzer, (8)---washing whizzer, (9)---first drying machine,
(10)---kibbler, (11)---calcium carbonate product, (12)---carbon dust cleaner,
(13)---the 3rd suction filter pump, (14)---carbon dust loft drier, (15)---carbon dust kibbler,
(16)---the carbon dust product, (17)---reactor drum, (18)---strainer,
(19)---second moisture eliminator, (20)---WHITE CARBON BLACK product, (21)---underpressure distillation device,
(22)---the sodium-chlor product.
Embodiment
Below in conjunction with specific embodiment the method for production superfine light calcium carbonate according to the invention and white carbon black coproduction sodium chloride and carbon dust is done and to be further described and to explain.
Embodiment one
With reference to Fig. 1, a kind of method of producing superfine light calcium carbonate and white carbon black coproduction sodium chloride and carbon dust, ammonium chloride mass content in the waste liquid of conversion couplet alkaline process generation earlier and the calcium hydroxide mass content in the carbide slag; Carbide slag and the waste associated alkali solution that will contain 500kg calcium hydroxide is to drop in corrosion-resistant reactor 1 at 1: 1.08 according to the pure substance mass ratio of calcium hydroxide and ammonium chloride, stirs, and reacts, and obtains containing the mixed solution of calcium chloride and ammoniacal liquor; With mixed solution warp first suction filter pump 2 suction filtrations that contain calcium chloride and ammoniacal liquor of gained, first whizzer 3 is centrifugal, obtains black carbon filter cake and clarifying liquid; The carbon filter cake of black is used to prepare carbon dust; Clarifying liquid drops in the carbonating tower 4; Using mass concentration is that 5% tensio-active agent emulsifiable concentrate is handled; Stir speed (S.S.) is 220r/min; Then feed dioxide gas and carry out carburizing reagent,, be the carbonization terminal point when reading is motionless to be zero when showing to go up with the carbonization terminal point of the said carburizing reagent of chlorination table 5 control; Carburizing reagent obtains the mixture of carbonated calcium deposit and ammonium chloride; Carbonated calcium and ammonium chloride mixt is centrifugal with 6 filtrations of second suction filter pump and second whizzer 7, obtain calcium carbonate filter cake and the solution that contains ammonium chloride; The gained calcium carbonate filter cake is warp washing whizzer 8 washing dehydrations successively, drying machine 9 dryings, and kibbler 10 is pulverized, and is packaged to be the calcium carbonate product 11 that contains 504.67kg lime carbonate; Said solution that contains ammonium chloride and water glass are to drop in reactor drum 17 at 1: 2.39 according to ammonium chloride and water glass pure substance mass ratio, under the stirring that blows slowly, carry out two hydrolysis reaction, and generate ammonia, WHITE CARBON BLACK and sodium-chlor; Ammonia is overflowed, and returns the utilization of system alkali systemic circulation; With strainer 18 filtering reaction products, obtain the solution of WHITE CARBON BLACK bullion and sodium chloride-containing; Said WHITE CARBON BLACK bullion obtains WHITE CARBON BLACK product 20 through second moisture eliminator, 19 dryings; The solution of said sodium chloride-containing is sent into to distill in the underpressure distillation device 21 and is obtained sodium-chlor product 22.
Said carbon filter cake and excessive hydrochloric acid excessive response in carbon dust cleaner 12 is removed the carbide slag that does not have complete reaction, through the 3rd suction filter pump 13 suction filtrations, obtains purified carbon dust; Said purified carbon dust through dehydration, dry in carbon dust loft drier 14, is crushed into carbon dust product 16 again in the carbon dust kibbler 15.
Embodiment two
With reference to Fig. 1, a kind of method of producing superfine light calcium carbonate and white carbon black coproduction sodium chloride and carbon dust, the mass content of the ammonium chloride in the conversion waste associated alkali solution and the mass content of the calcium hydroxide in the carbide slag earlier; Carbide slag and the waste associated alkali solution that will contain 500kg calcium hydroxide is to drop in corrosion-resistant reactor 1 at 1: 1.45 according to the pure substance mass ratio of calcium hydroxide and ammonium chloride, stirs, and reacts, and obtains containing the mixed solution of calcium chloride and ammoniacal liquor; With mixed solution warp first suction filter pump 2 suction filtrations that contain calcium chloride and ammoniacal liquor of gained, first whizzer 3 is centrifugal, obtains black carbon filter cake and clarifying liquid; The carbon filter cake of black is used to prepare carbon dust; Clarifying liquid drops in the carbonating tower 4; Using mass concentration is 8% surfactant treatment; Stir speed (S.S.) is 280r/min, and wherein containing mass concentration in the tensio-active agent and be 6% emulsifiable concentrate and mass concentration is 2% tween 80, and the mixed gas that then feeds carbon dioxide containing gas 25% carries out carburizing reagent; With the carbonization terminal point of the said carburizing reagent of chlorination table 5 control, be the carbonization terminal point when reading is motionless to be zero when showing to go up; Carburizing reagent obtains carbonated calcium deposit and ammonium chloride mixt; Carbonated calcium and ammonium chloride mixt is centrifugal with second suction filter pump 6 and second whizzer 7, obtain calcium carbonate filter cake and the solution that contains ammonium chloride; The gained calcium carbonate filter cake is warp washing whizzer 8 washing dehydrations successively, drying machine 9 dryings, and kibbler 10 is pulverized, and is packaged to be the calcium carbonate product 11 that contains 677.57kg lime carbonate; Said solution that contains ammonium chloride and water glass are to drop in reactor drum 17 at 1: 0.64 according to ammonium chloride and water glass pure substance mass ratio, under the stirring that blows slowly, carry out two hydrolysis reaction, and generate ammonia, WHITE CARBON BLACK and sodium-chlor; Ammonia is overflowed, and returns the utilization of system alkali systemic circulation; With strainer 18 filtering reaction products, obtain WHITE CARBON BLACK bullion and sodium chloride solution; Said WHITE CARBON BLACK bullion obtains WHITE CARBON BLACK product 20 through second moisture eliminator, 19 dryings; The solution of said sodium chloride-containing is sent into to distill in the underpressure distillation device 21 and is obtained sodium-chlor product 22.
Said carbon filter cake and excessive hydrochloric acid excessive response in carbon dust cleaner 12 is removed the carbide slag that does not have complete reaction, through the 3rd suction filter pump 13 suction filtrations, obtains purified carbon dust; Said purified carbon dust through dehydration, dry in carbon dust loft drier 14, is crushed into carbon dust product 16 again in the carbon dust kibbler 15.
Embodiment three
With reference to Fig. 1, a kind of method of producing superfine light calcium carbonate and white carbon black coproduction sodium chloride and carbon dust, the mass content of the ammonium chloride in the conversion waste associated alkali solution and the mass content of the calcium hydroxide in the carbide slag earlier; Carbide slag and the waste associated alkali solution that will contain 500kg calcium hydroxide is to drop in corrosion-resistant reactor 1 at 1: 1.32 according to the pure substance mass ratio of calcium hydroxide and ammonium chloride, stirs, and reacts, and generates the mixed solution that contains calcium chloride and ammoniacal liquor; With mixed solution warp first suction filter pump 2 suction filtrations that contain calcium chloride and ammoniacal liquor of gained, first whizzer 3 is centrifugal, obtains black carbon filter cake and clarifying liquid; The carbon filter cake of black is used to prepare carbon dust; Clarifying liquid drops in the carbonating tower 4; Using mass concentration is that 10% tensio-active agent tween 80 is handled; Stir speed (S.S.) is 320r/min; Then the mixed gas of carbon dioxide containing gas 40% carries out carburizing reagent, with the carbonization terminal point of the said carburizing reagent of chlorination table 5 control, is the carbonization terminal point when reading is motionless to be zero when showing to go up; Carburizing reagent obtains carbonated calcium deposit and ammonium chloride mixt; With the mixture of carbonated calcium deposit and ammonium chloride filter with second suction filter pump 6 and second whizzer 7 centrifugal, obtain the solution of carbonated calcium filter cake and ammonium chloride; The gained calcium carbonate filter cake is warp washing whizzer 8 washing dehydrations successively, drying machine 9 dryings, and kibbler 10 is pulverized, and is packaged to be the calcium carbonate product 11 of lime carbonate; Said solution that contains ammonium chloride and water glass are to drop in reactor drum 17 at 1: 1.50 according to ammonium chloride and water glass pure substance mass ratio, under the stirring that blows slowly, carry out two hydrolysis reaction, and generate ammonia, WHITE CARBON BLACK and sodium-chlor; Ammonia is overflowed, and returns the utilization of system alkali systemic circulation; With strainer 18 filtering reaction products, obtain the solution of WHITE CARBON BLACK bullion and sodium chloride-containing; Said WHITE CARBON BLACK bullion obtains WHITE CARBON BLACK product 20 through second moisture eliminator, 19 dryings; The solution of said sodium chloride-containing is sent into to distill in the underpressure distillation device 21 and is obtained sodium-chlor product 22.
Said carbon filter cake and excessive hydrochloric acid excessive response in carbon dust cleaner 12 is removed the carbide slag that does not have complete reaction, through the 3rd suction filter pump 13 suction filtrations, obtains purified carbon dust; Said purified carbon dust through dehydration, dry in carbon dust loft drier 14, is crushed into carbon dust product 16 again in the carbon dust kibbler 15.
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 (5)
1. method of producing superfine light calcium carbonate and white carbon black coproduction sodium chloride and carbon dust, the used starting material of this method are waste associated alkali solution and carbide slag, it is characterized in that, comprise the steps:
A: convert the mass content of the ammonium chloride in the waste associated alkali solution and the mass content of the calcium hydroxide in the carbide slag respectively;
B: is 1: 1.08～1.45 to drop in the corrosion-resistant reactors (1) carbide slag and waste associated alkali solution according to the pure substance mass ratio of calcium hydroxide and ammonium chloride, reacts, and obtains containing the mixed solution of calcium chloride and ammoniacal liquor;
C: with mixed solution warp first suction filter pump (2) suction filtration that contains calcium chloride and ammoniacal liquor of step B gained, first whizzer (3) is centrifugal, obtains black carbon filter cake and clarifying filtrating;
D: the clarifying filtrating of step C gained is dropped in the carbonating tower (4); Using mass concentration is that 5～10% tensio-active agents carry out surface treatment; Stir speed (S.S.) is 220～320r/min, then feeds dioxide gas and carries out carburizing reagent, obtains carbonated calcium deposit and ammonium chloride mixt;
E: the carbonated calcium deposit and the ammonium chloride mixt of step D gained is centrifugal with second suction filter pump (6) and second whizzer (7), obtain calcium carbonate filter cake and the solution that contains ammonium chloride;
F: with the calcium carbonate filter cake of step e gained successively through washing whizzer (8) washing dehydration, first drying machine (9) drying, kibbler (10) is pulverized, and is packaged to be calcium carbonate product (11);
G: is in 1: 0.64～2.39 input reactor drums (17) with the solution that contains ammonium chloride and the water glass of step e gained according to ammonium chloride and water glass pure substance mass ratio; Under the stirring that blows slowly, carry out two hydrolysis reaction; Generate ammonia, precipitation of silica, water and sodium-chlor;
H: the reaction product of step G gained is filtered through strainer (18), obtain the solution of WHITE CARBON BLACK bullion and sodium chloride-containing;
I: the WHITE CARBON BLACK bullion of step H gained obtains WHITE CARBON BLACK product (20) through second moisture eliminator (19) drying;
J: the solution of the sodium chloride-containing of step H gained is sent into to distill in the underpressure distillation device (21) and is obtained sodium-chlor product (22);
K: said carbon filter cake and excessive hydrochloric acid be excessive response in carbon dust cleaner (12), removes the carbide slag that does not have complete reaction, obtains purified carbon filter cake through the 3rd suction filter pump (13) suction filtration;
L: said purified carbon filter cake through dehydration, dry in carbon dust loft drier (14), is crushed into carbon dust product (16) again in the carbon dust kibbler (15).
2. the method for production superfine light calcium carbonate as claimed in claim 1 and white carbon black coproduction sodium chloride and carbon dust; It is characterized in that; With the carbonization terminal point of the said carburizing reagent of chlorination table (5) control, be the carbonization terminal point when reading is motionless to be zero among the step D when showing to go up.
3. the method for production superfine light calcium carbonate as claimed in claim 1 and white carbon black coproduction sodium chloride and carbon dust is characterized in that, the described dioxide gas of step D is pure carbon dioxide gas or carbonic acid gas volume content greater than 20% mixed gas.
4. the method for production superfine light calcium carbonate as claimed in claim 1 and white carbon black coproduction sodium chloride and carbon dust is characterized in that, said tensio-active agent is selected from emulsifiable concentrate, tween 80 and the mixture of the two.
5. the method for production superfine light calcium carbonate as claimed in claim 1 and white carbon black coproduction sodium chloride and carbon dust is characterized in that, said ammonia returns the utilization of system alkali systemic circulation.
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|---|---|---|---|---|
| US9902652B2 (en) | 2014-04-23 | 2018-02-27 | Calera Corporation | Methods and systems for utilizing carbide lime or slag |
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| RU2489355C2 (en) * | 2011-07-05 | 2013-08-10 | Алексей Гаврилович Мешандин | Method for synthesis of finely dispersed calcium carbonate |
| JP2023514456A (en) | 2020-02-25 | 2023-04-05 | アレラク， インコーポレイテッド | Method and system for processing lime to form vaterite |
| GB2613474A (en) | 2020-06-30 | 2023-06-07 | Arelac Inc | Methods and systems for forming vaterite from calcined limestone using electric kiln |
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| CN1058005A (en) * | 1991-08-15 | 1992-01-22 | 常州飞机制造厂技术开发服务部 | Method with preparing high-purity technical calcium carbonate from calcium carbide dregs |
| CN100424015C (en) * | 2004-12-20 | 2008-10-08 | 王嘉兴 | Method for fabricting Nano active calcium carbonate as well as carbon powder from carbide slag |
| EP1712523A1 (en) * | 2005-04-11 | 2006-10-18 | Omya Development AG | Precipitated calcium carbonate pigment, especially for use in inkjet printing paper coatings |
| CN100390064C (en) * | 2005-04-28 | 2008-05-28 | 卢忠远 | Production of superfine calcium carbonate from carbide slag |
| CN101580257A (en) * | 2009-04-08 | 2009-11-18 | 王嘉兴 | Method for preparing common active calcium carbonate series products and ammonium chloride by carbide slag |
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