CN1032912C - Process for preparing light calcium carbonate in form of flake crystal - Google Patents
Process for preparing light calcium carbonate in form of flake crystal Download PDFInfo
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- CN1032912C CN1032912C CN 93108625 CN93108625A CN1032912C CN 1032912 C CN1032912 C CN 1032912C CN 93108625 CN93108625 CN 93108625 CN 93108625 A CN93108625 A CN 93108625A CN 1032912 C CN1032912 C CN 1032912C
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- CN
- China
- Prior art keywords
- calcium carbonate
- light calcium
- crystal
- boride
- present
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- 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.)
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Abstract
The present invention relates to a method for preparing flaky crystal light calcium carbonate. The present invention adopts boride as crystal control agents, and prepares favorable flaky crystal light calcium carbonate with a liquid phase one-step carbonization method, and the boride as the crystal control agents adopted by the present invention has the advantages of low toxicity and low price. The present invention adopts the one-step production process, has the advantage of safe and convenient operation by operators, and is suitable for industrialization production.
Description
The present invention relates to a kind of preparation method of lamellar crystal light calcium carbonate.
Light calcium carbonate is widely used as filler in papermaking, plastics, rubber and coating.The lamellar crystal light filler can make the planeness on surface and smooth finish improve, and particularly in paper industry, can be used to replace the high territory of sheet, uses for surface applied when making fine paper.
The development of flake light calcium carbonate starts from the eighties.Because the stable crystal shape of lime carbonate generally is chain, spindle shape and cubic, rather than flaky, the most two step carborizations that adopt of therefore existing study route.Promptly at first in liquid phase with Ca (OH)
2Use CO
2Carbonization is arrived to a certain degree, flaky intermediate product is separated, under the condition of unlikely change crystal shape, finish the carburizing reagent of the second half again and produce lamellar crystal light calcium carbonate (the clear 58-193495 of Japanese Patent, clear 63-50316, clear 61-219715, clear 61-219717, German patent DE-3245103), because reactions steps was divided into for two steps, cause the technology of the complex process and the second step carbonization, energy consumption is more, so the two step method production technique has complex process, power consumption increases, cost rises shortcoming, so that fails industrialization so far.
Nineteen ninety Japanese Patent (flat 2-184519) proposes to use the method for crystal control agent organic phosphine, comes a step carbonization to produce flaky calcium carbonate.Concrete technology is (CaO+H in certain density lime milk solution
2O), feed the CO of certain flow rate
2, react and add organic phosphine after ten minutes, continue logical CO
2Complete to carbonization.Product after filtration, promptly to get diameter after the drying be that 1-2 μ, thickness are the light calcium carbonate of the platy particle of 0.1-0.2 μ.This technology is simple than two step method, has propagable basis, but because used crystal control agent organic phosphine costs an arm and a leg, toxicity is bigger, and see that from the appended electron micrograph of this patent specification prepared form of flake crystal lime carbonate sheet crystalline form is not ideal, so its industrial prospect and being far from good.
The objective of the invention is to do crystal control agent, with the good light calcium carbonate of liquid phase one-step Carbonization Preparation form of flake crystal with boride.
Technical scheme of the present invention is: proportioning according to dosage, in water, add CaO, and be made into lime milk solution, control to certain temperature, feed with certain flow CO
2, add the crystal control agent boride, continue to feed CO again
2, complete up to carbonization.Product after filtration, drying obtains lamellar crystal light calcium carbonate.
Employed crystal control agent boride in the above-mentioned technology can be boric acid, borax, Na
3B
3O
6, K
3B
3O
6, K
2[B
5O
6(OH)]
2H
2O, B
2H
6, HBO
2, B
2O
3, BX
3, its add-on is the 0.3%-3.5% of CaO amount.
Boride reaction begin and reaction process in add all can, to add effect in the reaction for well.
This temperature of reaction can be controlled in 0-25 ℃, CO
2Flow control is in every gram CaO0.2-1.2ml/ second, and lime milk concentration is a CaO3-18g/100ml water.
Effect of the present invention: the present invention adopts boride inexpensive, low toxicity to do crystal control agent, with liquid phase one-step Carbonization Preparation lamellar crystal light calcium carbonate, has operator's operational safety, easy advantage, and suitable suitability for industrialized production.The stereoscan photograph of the form of flake crystal lime carbonate by the present invention preparation sees that the form of flake crystal of this lime carbonate is good, and is more effective than the stereoscan photograph of the light calcium carbonate of producing as crystal control agent with the Japanese Patent organic phosphine.
The lamellar crystal light CaCO of Fig. 1, Japanese Patent (flat 2-184519) preparation
3Stereoscan photograph.
Fig. 2, the lamellar crystal light CaCO that uses the present invention (embodiment 1) to prepare
3Stereoscan photograph.
Embodiment 1:
Preparation concentration is the milk of lime 150ml of 10 gram CaO/100ml water, when treating that temperature drops to 18 ℃, and logical CO
2, speed is 0.5ml/ second.Initial specific conductivity is 7.2 * 10
3μ S/cm, reaction adds 0.1 gram H after half an hour
3BO
3, continue logical CO
2Reduce to 1 * 10 up to specific conductivity
3μ S/gm, 2 hours 40 minutes reaction times product filters, and gets 25 grams after 100 ℃ of following dryings.Use the sem observation crystalline form, as shown in Figure 2.Its average grain diameter is 1-2 μ, and the ratio that sheet footpath and sheet are thick is 5: 1 to 10: 1.
Comparative example 1:
Remove and do not add H
3BO
4Outward, other condition is identical with embodiment 1.In 3 hours reaction times, product weighs 25 grams, and electron scanning micrograph shows that majority is granular and the cubic crystal.
Embodiment 2:
CaO600g is incorporated in 6 premium on currency, treats to lead to when temperature is reduced to 20 ℃ CO
2, flow is 0.17M
3/ h, reaction adds 10 gram H after half an hour
3BO
3, continue logical CO
2, make specific conductivity by initial 5.8 * 10
3μ S/cm reduces to less than 1 * 10
3μ S/cm gets 1 kilogram in lime carbonate.Electron scanning micrograph shows that crystal is the sheet Polygons, mean diameter 1 μ, and the 5 thick ratios in sheet footpath were greater than 10: 1.
Embodiment 3:
Add 8 gram CaO and do in the 100ml water, when treating that temperature is reduced to 15 ℃, logical CO
2Flow is 0.6ml/ second, and initial specific conductivity is 6.2 * 10
3μ S/cm reacts and adds 0.2 gram borax after 20 minutes, continues logical CO
2Up to specific conductivity less than 1 * 10
3μ S/cm.2 hours 10 minutes reaction times.Product filters, drying.Electron scanning micrograph shows that crystal is the sheet Polygons, mean diameter 2 μ, and the ratio that sheet footpath and sheet are thick is 5: 1 to 8: 1.
Claims (2)
1. one kind by with crystal control agent and adopt the method for liquid phase one-step Carbonization Preparation lamellar crystal light calcium carbonate, and the proportioning of CaO and water is at 3-18g/100ml water, and temperature of reaction is controlled at 0-25 ℃, CO
2Flow control adds crystal control agent in every gram CaO0.2-1.2ml/ second, continues to feed CO again
2, complete up to carbonization, product is after filtration, drying obtains lamellar crystal light calcium carbonate, and it is characterized in that: used crystal control agent is a boride.
2. preparation method according to claim 1 is characterized in that: boride can be boric acid, borax, Na
3B
3O
6, K
3B
3O
6, K
2[B
5O
8(OH)]
2H
2O, B
2H
6, HBO
2, B
2O
3, BX
3, its add-on is the 0.3%-3.5% of CaO amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93108625 CN1032912C (en) | 1993-07-15 | 1993-07-15 | Process for preparing light calcium carbonate in form of flake crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93108625 CN1032912C (en) | 1993-07-15 | 1993-07-15 | Process for preparing light calcium carbonate in form of flake crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1080909A CN1080909A (en) | 1994-01-19 |
| CN1032912C true CN1032912C (en) | 1996-10-02 |
Family
ID=4987211
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93108625 Expired - Fee Related CN1032912C (en) | 1993-07-15 | 1993-07-15 | Process for preparing light calcium carbonate in form of flake crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1032912C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2002359958A1 (en) * | 2001-12-31 | 2003-07-15 | Beijing University Of Chemical Technology | Calcium carbonate of different shapes and the preparing process thereof |
| CN100400422C (en) * | 2005-12-29 | 2008-07-09 | 上海耀华纳米科技有限公司 | Plate-like light calcium carbonate and preparation technology thereof |
| CN100467381C (en) * | 2006-12-25 | 2009-03-11 | 上海东升新材料有限公司 | Flake light calcium carbonate and its preparing method and application |
| CN100567407C (en) * | 2007-06-28 | 2009-12-09 | 中国科学院上海硅酸盐研究所 | Nano layered calcium carbonate base bionic composite material and synthetic method thereof |
| CN105883880A (en) * | 2016-04-07 | 2016-08-24 | 安徽江东科技粉业有限公司 | Preparation method of sheet superfine calcium carbonate for paper coating |
| CN109667189B (en) * | 2017-10-13 | 2022-07-26 | 东升新材料（山东）有限公司 | Preparation method of chrysanthemum-shaped light calcium carbonate filler |
| CN109667190B (en) * | 2017-10-13 | 2022-04-01 | 东升新材料（山东）有限公司 | Cubic light calcium carbonate filler composition and preparation method and application thereof |
| CN109665553B (en) * | 2017-10-13 | 2022-04-01 | 东升新材料（山东）有限公司 | Preparation method of cubic light calcium carbonate filler |
-
1993
- 1993-07-15 CN CN 93108625 patent/CN1032912C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1080909A (en) | 1994-01-19 |
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