CN103523813A - Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water - Google Patents
Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water Download PDFInfo
- Publication number
- CN103523813A CN103523813A CN201310498192.9A CN201310498192A CN103523813A CN 103523813 A CN103523813 A CN 103523813A CN 201310498192 A CN201310498192 A CN 201310498192A CN 103523813 A CN103523813 A CN 103523813A
- Authority
- CN
- China
- Prior art keywords
- calcium carbonate
- water
- temperature
- nano
- suspension
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to an industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water, and is used for solving a problem that a nano calcium carbonate product is poor in repeatability and unstable in quality after the existing water treatment technology is utilized to treat the filter-pressing water in an existing preparation method. The industrial preparation method comprises the following steps: filtering the filter-pressing water in a nano calcium carbonate producting process by using a high temperature resistant filter press, keeping the water temperature at 65 DEG C-85 DEG C, modulating the mass concentration of digested calcium hydroxide liquor to 6%-10%, and controlling the temperature to 22 DEG C-35 DEG C; then, filling into a reaction kettle, regulating the temperature of Ca(OH)2 suspension liquid to 25 DEG C-40 DEG C; ventilating a gas mixture of carbon dioxide and nitrogen gas into a carbonization reaction kettle at the velocity of 0.6-0.8 cubic meter/second, adding a dispersing agent which accounts for 0.02%-0.05% of the total weight of the Ca(OH)2 in the suspension liquid of the Ca(OH)2, heating a nano calcium carbonate sizing agent to 55 DEG C-65 DEG C, and adding a coating agent. The industrial preparation method disclosed by the invention realizes the closed cycle of nano calcium carbonate process water.
Description
Technical field
The present invention relates to a kind of preparation method of calcium carbonate, particularly the industrial production process of nano-calcium carbonate is produced in a kind of press filtration water reuse that utilizes production nano-calcium carbonate to produce.
Background technology
Nano-calcium carbonate refers to that particle diameter is less than the superfine powder of 100 nanometers, and nm-class active calcium carbonate refers to that calcium carbonate becomes oil loving Chemicals by wetting ability after surperficial organic process, and product can be widely used in the industries such as vehicle paint base, rubber, plastics.Super-refinement, narrow diameter distribution, crystal morphology stablize and product quality circulation ratio height is a basic demand of this product.Existing nano-calcium carbonate is produced technical process: limestone calcination produces lime and carbonic acid gas, lime is digested to certain density slurries under certain processing condition, add certain additive, pass into carbonic acid gas and control the calcium carbonate serosity that certain carbonization technique parameter carbonization forms certain crystalline form and pattern, carry out after surface modification, through press filtration, dry, pulverize, packing forms calcium carbonate finished product.In said process, in lime slaking operation, the general fresh water that adopts is as process water, and the feature of the water producing through press filtration operation is: temperature is high, is generally 80-85 degree, COD is high, indicator of suspended solids fluctuation is large, the fluctuation of direct reuse product index is large.At present, large multiple enterprises reaches press filtration water treatment the emission standard discharge of regulation, some repay examination to have Some Enterprises to carry out technology to the closed cycle of water, and main technological line has following two kinds: the one, and utilize traditional water technology to process extremely middle water reuse standard and carry out reuse.Main technological line has: flocculation+filtration+biochemical process, membrane processing method.The feature of this technological line is: introduced organic-inorganic flocculation agent, water temperature can not surpass 35 degree, and the yield of water is generally between 65%-80%.The 2nd, water is produced for the not high calcium carbonate of quality requirements.The problem that existing water technology exists is: the one, and the wasting of resources, the component substance basis of heat and formation COD is removed or loses as refuse; The 2nd, the waste of water is serious; The 3rd, cost of water treatment is high; The 4th, because the flocculation agent of introducing in its treating processes is as close with the character of calcium in magnesium, aluminium etc., calcium carbonate crystal process is impacted.Cause the poor reproducibility of nano-calcium carbonate product quality, the unsettled problem of product quality.
Summary of the invention
The invention provides the industrial production process of the aquatic product nano-calcium carbonate of a kind of reuse press filtration, having solved press filtration water that production process that existing preparation method exists produces can not reuse and utilize poor reproducibility and the unsettled problem of product quality of the nano-calcium carbonate product quality existing after the reuse of existing water technology processing press filtration water.
The present invention solves above technical problem by the following technical programs:
An industrial production process for the aquatic product nano-calcium carbonate of reuse press filtration, comprises the following steps:
The first step, by high temperature resistant selectivity, see through film the press filtration water of producing in nano-calcium carbonate process is filtered;
Second step, the water after the first step is filtered carry out cascade filtration through Self-cleaning filter, remove suspended substance; More than water temperature after processing remains on 75 degree.
The 3rd step, water that second step is obtained by water examination standard test after for lime slaking, and to keep water temperature be 65-85 degree, the mass concentration of postdigestive aqua calcis is controlled at 11-17%;
The 4th step, the postdigestive aqua calcis of the 3rd step is modulated into mass concentration is 6-10%, and temperature is controlled at 22-35 degree, then packs in reactor, and loadings is the 60%-80% of reactor volume;
The 5th step, adjustment Ca (OH)
2the temperature of suspension is to 25-40 ℃;
The 6th step, with the speed of 0.6-0.8 cube of meter per second to the mixed gas that passes into carbonic acid gas and nitrogen in carburizing reagent still, in the volumetric concentration of this carbon dioxide in gas mixture gas, be 35%-60%, with Ca (OH)
2the mass concentration of suspension is that benchmark goes out Ca (OH)
2total mass, as Ca (OH)
2the Ca (OH) of participation and carbon dioxide reaction in suspension
2quality reach Ca (OH)
2the 8-10% of total mass time, add Ca (OH)
2the crystal structure adjusting agent of 0.5-2% of total mass, continue carbonization, until Ca (OH)
2the pH value of suspension reaches 6-7.5, generates nano level calcite, and temperature of reaction is controlled at 50-65 ℃;
The 7th step, at Ca (OH)
2suspension in add Ca (OH)
2the dispersion agent of 0.2-0.5 ‰ of total mass, adjust the surface charge of nanoparticle, dispersion agent forms electrostatic double layer on calcium carbonate surface;
The 8th step, one or both in lipid acid or water soluble peptide acid esters coupling agent are configured to aqueous solution coating, said lipid acid is C
12-C
18lipid acid, water-soluble metatitanic acid fat coupling agent is one or more in CT-54 coupling agent, propionic acid titanium CT-64 coupling agent or hydramine lipid acid titanium coupling agent; Lipid acid or water-soluble carbon acid esters coupling agent are configured to the aqueous solution coating that concentration is 10-20%;
The 9th step, nano-calcium carbonate slurry is heated to 75-85 ℃, then adds coating, the add-on of coating is counted 0.5-5% with the weight of calcium carbonate, and the coated treatment time is 1-3 hour, obtains nm-class active calcium carbonate.
Said crystal structure adjusting agent is a kind of or its mixture in phosphoric acid salt, vitriol, acetate, Citrate trianion, monose or polysaccharide.
Said dispersion agent is one or more mixtures of chloride salt, polyacrylate.
Synthetic nm-class active calcium carbonate particle is controlled between 50-80nm as stated above, cube, and specific surface area is greater than 24m
2/ g, oil-absorption(number) is less than 27g/100gCaOC3, and good dispersity, without agglomeration, can be used as the functional stuffing of high-grade rubber, plastics and vehicle paint base.Adopt present method, 20% of the generated time that generated time is the production of the band stirring carbonization at low temperature precipitator method, product repetition rate reaches 99%.
The present invention adopts water conditioning and production technique adjustment to combine, and optionally process water is processed, and has formed a kind of nano-calcium carbonate production method of efficient, energy-conservation, comprehensive utilization of resources, has realized the closed cycle of nano-calcium carbonate process water.Preparation method of the present invention draws the advantage that stirs the carbonization precipitator method, according to the ultimate principle of crystallography, introduce brilliant control agent and dispersion agent, significantly increase the carbonic acid gas tolerance that participates in reaction, searching out under a kind of and high speed of response utilizes press filtration backwater to produce nano-calcium carbonate production method, compare with traditional nano-calcium carbonate production technique, the method speed of response is high, reaction finishing temperature is high, reaction times is short, the water of production process, heat, compound are fully utilized, and product quality repetition rate is high, and reaction unit industrialization realizes easily.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment mono-:
The first step, in being the carburizing reagent still of 3 meters high 6 meters, diameter adds 40 cubes with the Ca (OH) of press filtration water digestion
2suspension, Ca (OH)
2the mass concentration of suspension is 7.92%.
Second step,, adjust Ca (OH)
2the temperature to 24 of suspension ℃;
The 3rd step, with the speed of 0.6 cube of meter per second to the mixed gas that passes into carbonic acid gas and nitrogen in reactor, the volumetric concentration of carbon dioxide in gas mixture gas is 35%, through 10 minutes, as Ca (OH)
2when the carbonation rate of suspension reaches 8-10%, add the polysaccharide of 35 kilograms, continue carbonization, until Ca (OH)
2the pH value 6.85 of suspension, generates nano level calcite, and reaction finishing temperature is 61 ℃.
The 4th step, at Ca (OH)
2suspension in add the polyacrylate of 10 kilograms;
The 5th step, 225 kilograms of lipid acid are configured to 10% aqueous solution coating;
The 6th step, nano-calcium carbonate slurry is heated to 85 ℃, then adds coating, the coated treatment time is 4 hours, obtains nm-class active calcium carbonate.
Embodiment bis-:
The first step, in being the carburizing reagent still of 3 meters high 6 meters, diameter adds the Ca (OH) of 30 cubes
2suspension, Ca (OH)
2the mass concentration of suspension is 7.92%;
Second step, adjustment Ca (OH)
2the temperature to 24 of suspension ℃;
The 3rd step, with the speed of 0.7 cube of meter per second to the mixed gas that passes into carbonic acid gas and nitrogen in reactor, the volumetric concentration of carbon dioxide in gas mixture gas is 52%, through 10 minutes, as Ca (OH)
2when the carbonation rate of suspension reaches 8-10%, add the polysaccharide of 25Kg, continue carbonization, until Ca (OH)
2the pH value 6.85 of suspension, generates nano level calcite, and reaction finishing temperature is 61 ℃.
The 4th step, at Ca (OH)
2suspension in add 12Kg polyacrylate;
The 5th step, 166 kilograms of lipid acid are configured to 10% aqueous solution coating;
The 6th step, nano-calcium carbonate slurry is heated to 85 ℃, then adds coating, the coated treatment time is 4 hours, obtains nm-class active calcium carbonate.
Claims (3)
1. an industrial production process for the aquatic product nano-calcium carbonate of reuse press filtration, comprises the following steps:
The first step, by high temperature resistant selectivity, see through film the press filtration water of producing in nano-calcium carbonate process is filtered;
Second step, the water after the first step is filtered carry out cascade filtration through Self-cleaning filter, remove suspended substance; More than water temperature after processing remains on 75 degree;
The 3rd step, water that second step is obtained by water examination standard test after for lime slaking, and to keep water temperature be 65-85 degree, the mass concentration of postdigestive aqua calcis is controlled at 11-17%;
The 4th step, the postdigestive aqua calcis of the 3rd step is modulated into mass concentration is 6-10%, and temperature is controlled at 22-35 degree, then packs in reactor, and loadings is the 60%-80% of reactor volume;
The 5th step, adjustment Ca (OH)
2the temperature of suspension is to 25-40 ℃;
The 6th step, with the speed of 0.6-0.8 cube of meter per second to the mixed gas that passes into carbonic acid gas and nitrogen in carburizing reagent still, in the volumetric concentration of this carbon dioxide in gas mixture gas, be 35%-60%, with Ca (OH)
2the mass concentration of suspension is that benchmark goes out Ca (OH)
2total mass, as Ca (OH)
2the Ca (OH) of participation and carbon dioxide reaction in suspension
2quality reach Ca (OH)
2the 8-10% of total mass time, add Ca (OH)
2the crystal structure adjusting agent of 0.5-2% of total mass, continue carbonization, until Ca (OH)
2the pH value of suspension reaches 6-7.5, generates nano level calcite, and temperature of reaction is controlled at 50-65 ℃;
The 7th step, at Ca (OH)
2suspension in add Ca (OH)
2the dispersion agent of 0.2-0.5 ‰ of total mass, adjust the surface charge of nanoparticle, dispersion agent forms electrostatic double layer on calcium carbonate surface;
The 8th step, one or both in lipid acid or water soluble peptide acid esters coupling agent are configured to aqueous solution coating, said lipid acid is C
12-C
18lipid acid, water-soluble metatitanic acid fat coupling agent is one or more in CT-54 coupling agent, propionic acid titanium CT-64 coupling agent or hydramine lipid acid titanium coupling agent; Lipid acid or water-soluble carbon acid esters coupling agent are configured to the aqueous solution coating that concentration is 10-20%;
The 9th step, nano-calcium carbonate slurry is heated to 75-85 ℃, then adds coating, the add-on of coating is counted 0.5-5% with the weight of calcium carbonate, and the coated treatment time is 1-3 hour, obtains nm-class active calcium carbonate.
2. the industrial production process of the aquatic product nano-calcium carbonate of a kind of reuse press filtration according to claim 1, is characterized in that, said crystal structure adjusting agent is a kind of or its mixture in phosphoric acid salt, vitriol, acetate, Citrate trianion, monose or polysaccharide.
3. the industrial production process of the aquatic product nano-calcium carbonate of a kind of reuse press filtration according to claim 1, is characterized in that, said dispersion agent is one or more mixtures of chloride salt, polyacrylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310498192.9A CN103523813A (en) | 2013-10-22 | 2013-10-22 | Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310498192.9A CN103523813A (en) | 2013-10-22 | 2013-10-22 | Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103523813A true CN103523813A (en) | 2014-01-22 |
Family
ID=49926236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310498192.9A Pending CN103523813A (en) | 2013-10-22 | 2013-10-22 | Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103523813A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804473A (en) * | 2015-04-30 | 2015-07-29 | 建德市双超钙业有限公司 | Production method of special nano calcium carbonate for dual-component high-extrudability building silicone adhesive |
| EP2939980A1 (en) * | 2014-04-30 | 2015-11-04 | Omya International AG | Production of precipitated calcium carbonate |
| CN110697754A (en) * | 2019-10-31 | 2020-01-17 | 山西兰花华明纳米材料股份有限公司 | Method for preparing industrial precipitated calcium carbonate by recycling nano calcium carbonate filter pressing water |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4888160A (en) * | 1985-12-20 | 1989-12-19 | J.M. Huber Corporation | Process for producing calcium carbonate and products thereof |
| CN101525147A (en) * | 2008-12-04 | 2009-09-09 | 兰州理工大学 | Preparation method of nano calcium carbonate |
| CN101914312A (en) * | 2010-08-20 | 2010-12-15 | 常州碳酸钙有限公司 | Preparation method of nano activated calcium carbonate for coating |
| WO2012126594A1 (en) * | 2011-03-18 | 2012-09-27 | Ecoloop Gmbh | Method for the continuous production of precipitated calcium carbonate |
| CN203159368U (en) * | 2013-04-03 | 2013-08-28 | 中冶长天国际工程有限责任公司 | Wastewater treatment system for nano calcium carbonate production |
-
2013
- 2013-10-22 CN CN201310498192.9A patent/CN103523813A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4888160A (en) * | 1985-12-20 | 1989-12-19 | J.M. Huber Corporation | Process for producing calcium carbonate and products thereof |
| CN101525147A (en) * | 2008-12-04 | 2009-09-09 | 兰州理工大学 | Preparation method of nano calcium carbonate |
| CN101914312A (en) * | 2010-08-20 | 2010-12-15 | 常州碳酸钙有限公司 | Preparation method of nano activated calcium carbonate for coating |
| WO2012126594A1 (en) * | 2011-03-18 | 2012-09-27 | Ecoloop Gmbh | Method for the continuous production of precipitated calcium carbonate |
| CN203159368U (en) * | 2013-04-03 | 2013-08-28 | 中冶长天国际工程有限责任公司 | Wastewater treatment system for nano calcium carbonate production |
Non-Patent Citations (1)
| Title |
|---|
| 朱浩存: "纳米碳酸钙行业污染最小化技术", 《化工新型材料》, vol. 41, no. 7, 31 July 2013 (2013-07-31), pages 45 - 47 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2939980A1 (en) * | 2014-04-30 | 2015-11-04 | Omya International AG | Production of precipitated calcium carbonate |
| WO2015166090A1 (en) * | 2014-04-30 | 2015-11-05 | Omya International Ag | Production of precipitated calcium carbonate |
| CN106458624A (en) * | 2014-04-30 | 2017-02-22 | 欧米亚国际集团 | Production of precipitated calcium carbonate |
| US10000388B2 (en) | 2014-04-30 | 2018-06-19 | Omya International Ag | Production of PCC |
| CN104804473A (en) * | 2015-04-30 | 2015-07-29 | 建德市双超钙业有限公司 | Production method of special nano calcium carbonate for dual-component high-extrudability building silicone adhesive |
| CN110697754A (en) * | 2019-10-31 | 2020-01-17 | 山西兰花华明纳米材料股份有限公司 | Method for preparing industrial precipitated calcium carbonate by recycling nano calcium carbonate filter pressing water |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100455515C (en) | Method for preparing nano calcium carbonate particle | |
| TWI406814B (en) | Process for preparing surface-reacted calcium carbonate and its use | |
| CN108117055B (en) | Preparation method and production device of battery-grade iron phosphate | |
| CN102757075B (en) | Method for preparing calcium carbonate powders of different structures and shapes | |
| CN1807263A (en) | Method for producing iron oxide black using desilicified mud cake | |
| CN101177289A (en) | Method for preparing fibrous nano magnesium hydrate | |
| CN102701255A (en) | Method for high-concentration carbonization production of spherical nano calcium carbonate | |
| CN101935866B (en) | Method for preparing flaky calcite calcium carbonate crystal | |
| CN103922378A (en) | Method for preparing high-purity metastable vaterite calcium carbonate from gypsum | |
| CN103523813A (en) | Industrial preparation method of producing nano calcium carbonate by recycling filter-pressing water | |
| CN102976462B (en) | Preparation method of inorganic polymeric flocculant titanium tetrachloride | |
| CN104263014A (en) | Preparing method of high-purity active calcium carbonate used for coating | |
| CN101914312B (en) | Preparation method of nano activated calcium carbonate for coating | |
| CN101318682A (en) | Stephanoporate calcium carbonate, preparing method and application thereof | |
| CN100372773C (en) | Method for producing nano calcium carbonate particles for printing ink | |
| CN105214644B (en) | Modified titanium and its preparation method and application | |
| CN109692648A (en) | The adsorbent and preparation method thereof of sulfate ion in efficient absorption water | |
| CN103508479A (en) | Production method of nanometer calcium carbonate for electronic glue | |
| CN101913640B (en) | Method for preparing superfine activated calcium carbonate | |
| CN112939049A (en) | Method for preparing calcium sulfate by using acid-containing wastewater of titanium dioxide | |
| CN105271344B (en) | A kind of preparation method of strobile pattern calcite type micron order calcium carbonate granule | |
| CN108314240A (en) | A kind for the treatment of process of iron oxide red mother liquor | |
| CN109502656B (en) | Spherical Co (II) Co (III) hydrotalcite-like material and preparation method thereof | |
| CN110980679A (en) | Preparation method of spheroidal low-sulfur iron phosphate | |
| CN1204054C (en) | Grain size adjustable spherical chromium oxide superfine powder preparing method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140122 |