CN1490248A - Preparing method for chain superfine hydrofil - Google Patents
Preparing method for chain superfine hydrofil Download PDFInfo
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- CN1490248A CN1490248A CNA021311765A CN02131176A CN1490248A CN 1490248 A CN1490248 A CN 1490248A CN A021311765 A CNA021311765 A CN A021311765A CN 02131176 A CN02131176 A CN 02131176A CN 1490248 A CN1490248 A CN 1490248A
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- cao
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Abstract
A process for preparing superfine chain-shaped calcium carbonate features use of the composite form controlling agent composed of 3 assistants, and one-step carbonization reaction by intermittent bubbling. The resultant calcium carbonate has 20 nm for axial size and 11:1 for length to diameter ratio.
Description
Technical field
The present invention relates to a kind of preparation method of chain pattern calcium carbonate superfine powder.
Background technology
Chain superfine hydrofil is the nano-calcium carbonate calcium product with one dimension shape characteristic.Compare with fine particle calcium carbonate with traditional coarse whiting, chain superfine hydrofil has good strengthening action to natural rubber, synthetic rubber, can partly replace carbon black or white carbon black as reinforced filling, reduce cost greatly, and chain lime carbonate is during as the additive of coating, papermaking, plastics industry, show excellent performance equally, be with a wide range of applications.
Japanese Patent is more common in research about chain lime carbonate preparation technology, Japanese Patent (clear 45-31851, clear 47-22944, clear 50-33995) generally takes to add specific opportunity the method control shape and appearance of calcium carbonate of soluble salts such as sulfuric acid, sal epsom, calcium sulfate, the more about 30～40nm of the axial dimension of product in certain of carbonization process.Japanese Patent (clear 56-26613) adopts two step charrings, at first behind adding EDTA2Na or other organic acids, begins charing before reaction, stops charing when reaction proceeds to certain specified phase; Add a certain amount of soluble inorganic salt, behind the thorough mixing, continue to feed CO
2, beginning second charing stage finishes until charing.The length-to-diameter ratio of product increases, and axial dimension can be decreased to below the 20nm, but because carbonization process is finished in two steps, is unfavorable for the raising of production efficiency.
Summary of the invention
Purpose of the present invention is to adopt a step charring, is the morphology control agent with the combined additive of document different from the past, prepares and the similar chain superfine hydrofil product of Japanese Patent (clear 56-26613) effect.
Technical scheme of the present invention is: the CaO of doses ratio is prepared into lime slurry, behind the adding component A thorough mixing, under the certain temperature, feeds the CO of certain flow
2Gas adds an amount of B component and the agent of component C morphology control suitable opportunity at twice, logical continuously CO
2To the reaction end.Product after filtration, drying obtains chain superfine hydrofil.
Employed morphology control agent is in the above-mentioned technology: component A can be EDTA2Na, Ba Dousuan, toxilic acid, oxyacetic acid, phenylformic acid, B component can be AE0-3, PVP, Span20, Span40, Span60, DP-S81, Telo-70, and component C can be CaCl
2, CaSO
4, Ca (NO)
2, Ca
3(PO
4)
2, MgCl
2, MgSO
4, AlCl
3
Combined additive can together add, but component A adds before reaction, and B component and component C add effect respectively in reaction process best.
Temperature of reaction is controlled at 5～30 ℃, CO
2Flow is 12～24ml/min/g CaO, and lime milk concentration is 3～15g CaO/100ml H
2O.
Effect of the present invention: the present invention adopts combined additive, with intermittence the bubbling charring shape and appearance of calcium carbonate is controlled, carbonization process one step finishes, and has advantages of nontoxic raw materials, operational safety, easy advantage, is fit to suitability for industrialized production.From electromicroscopic photograph, the length-to-diameter ratio of this calcium carbonate product, and axial dimension suitable substantially with Japanese Patent (clear 56-26613).
Description of drawings
Fig. 1, the transmission electron microscope photo of the chain superfine hydrofil of embodiment 1.
Fig. 2, the transmission electron microscope photo of comparative example 1.
Fig. 3, the transmission electron microscope photo of comparative example 2.
Embodiment
Embodiment 1:
The preparation solid content is 5gCaO/100mlH
2The milk of lime 100ml of O, controlled temperature is 23 ℃, be reflected at beginning before, 0.34g EDTA2Na is dissolved in the 10ml water, add reaction system, stir that the flow with 65～70mL/min feeds CO behind the 40min
2Gas, the aqueous solution 4ml that adding contained 0.055g PVP dispersion agent when reaction proceeded to 15min add the CaCl of 0.025g/nL in reaction system when reaction proceeds to 40min
2Aqueous solution 2mL reacts some end to pH6～7.XRD analysis shows, gained CaCO
3Be the calcite phase.Obtain chain superfine hydrofil after 100 ℃ of dryings, transmission electron microscope photo as shown in Figure 1, its axial dimension is about 20nm, about 11: 1 of length-to-diameter ratio.
Comparative example 1:
Do not add PVP and CaCl
2, only adding EDTA2Na, other conditions are identical with embodiment 1, then lime carbonate still has the one dimension shape characteristic, transmission electron microscope photo as shown in Figure 2, its axial diameter is about 40～60nm, length-to-diameter ratio is about 6～7: 1, and axial dimension is big than embodiment 1, and major diameter comparing embodiment 1 is little.
Comparative example 2:
Only add EDTA2Na and CaCl
2, do not add PVP, other conditions are identical with embodiment 1, the transmission electron microscope photo of gained calcium carbonate product as shown in Figure 3, the about 30nm of its axial diameter, about 4: 1 of length-to-diameter ratio.Axial dimension is little than comparative example 1, reduces but length-to-diameter ratio is also corresponding.
Embodiment 2:
The preparation solid content is 5gCaO/100mlH
2The milk of lime 100ml of O, controlled temperature is 23 ℃, be reflected at beginning before, 0.34g EDTA2Na is dissolved in the 10ml water, add reaction system, stir that the flow with 65～70mL/min feeds CO behind the 40min
2Gas adds 1ml AE0-3 dispersion agent 1ml when reaction proceeds to 1 5min, add the CaCl of 0.025g/mL when reaction proceeds to 40min
2Aqueous solution 2mL reacts some end to pH6～7.Obtain chain superfine hydrofil after 100 ℃ of dryings, its axial dimension is about 30nm, about 10: 1 of length-to-diameter ratio, but its dispersion effect is not as good as embodiment 1.
Claims (4)
1, a kind of morphology control agent by combination, with intermittence the bubbling charring prepare the method for the good chain superfine hydrofil of dispersion effect.The CaO of doses ratio is prepared into lime slurry, under the certain temperature, feeds the CO of certain flow
2Gas adds an amount of morphology control agent suitable opportunity respectively, logical continuously CO
2To the reaction end.Product after filtration, drying obtains chain superfine hydrofil.It is characterized in that: carbonization process need not to interrupt, and a step finishes, and the shape characteristic of lime carbonate is realized by the Combination Control of three kinds of additives.
2, preparation method according to claim 1, it is characterized in that: crystal morphology is finished by the Combination Control of additive, this Combination Control agent is made of two or more component, component A can be EDTA2Na, Ba Dousuan, toxilic acid, oxyacetic acid, phenylformic acid, B component can be AE0-3, PVP, Span20, Span40, Span60, DP-S81, Telo-70, and component C can be CaCl
2, CaSO
4, Ca (NO
3)
2, Ca
3(PO
4)
2, MgCl
2, MgSO
4, AlCl
3
3, according to the described preparation method of claim 1, it is characterized in that: the Combination Control agent can be component A, B, a kind of among the C, two or three, wherein the add-on of component A is more than 0.5% of CaO, and the add-on of B component is more than 0.5% of CaO, and the add-on of component C is more than 0.5% of CaO.
4, preparation method according to claim 1 is characterized in that: combined additive can together add, but component A adds before reaction, and B component and component C add effect respectively in reaction process best.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021311765A CN1490248A (en) | 2002-10-15 | 2002-10-15 | Preparing method for chain superfine hydrofil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA021311765A CN1490248A (en) | 2002-10-15 | 2002-10-15 | Preparing method for chain superfine hydrofil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1490248A true CN1490248A (en) | 2004-04-21 |
Family
ID=34144819
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA021311765A Pending CN1490248A (en) | 2002-10-15 | 2002-10-15 | Preparing method for chain superfine hydrofil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668602A (en) * | 2016-04-07 | 2016-06-15 | 安徽江东科技粉业有限公司 | Preparation method for calcium carbonate superfine powder |
| CN105776301A (en) * | 2016-04-07 | 2016-07-20 | 安徽江东科技粉业有限公司 | Preparing method of porous calcium carbonate |
| CN105883881A (en) * | 2016-04-07 | 2016-08-24 | 安徽江东科技粉业有限公司 | Preparation method of superfine calcium carbonate for printing ink |
| CN108069452A (en) * | 2017-12-19 | 2018-05-25 | 安徽省宣城市华纳新材料科技有限公司 | A kind of preparation method of chain calcite type calcium carbonate |
| CN110980787A (en) * | 2019-12-25 | 2020-04-10 | 广西华纳新材料科技有限公司 | Preparation method of calcium carbonate-calcium sulfate nano composite chain material |
-
2002
- 2002-10-15 CN CNA021311765A patent/CN1490248A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668602A (en) * | 2016-04-07 | 2016-06-15 | 安徽江东科技粉业有限公司 | Preparation method for calcium carbonate superfine powder |
| CN105776301A (en) * | 2016-04-07 | 2016-07-20 | 安徽江东科技粉业有限公司 | Preparing method of porous calcium carbonate |
| CN105883881A (en) * | 2016-04-07 | 2016-08-24 | 安徽江东科技粉业有限公司 | Preparation method of superfine calcium carbonate for printing ink |
| CN108069452A (en) * | 2017-12-19 | 2018-05-25 | 安徽省宣城市华纳新材料科技有限公司 | A kind of preparation method of chain calcite type calcium carbonate |
| CN110980787A (en) * | 2019-12-25 | 2020-04-10 | 广西华纳新材料科技有限公司 | Preparation method of calcium carbonate-calcium sulfate nano composite chain material |
| CN110980787B (en) * | 2019-12-25 | 2022-07-19 | 广西华纳新材料股份有限公司 | Preparation method of calcium carbonate-calcium sulfate nano composite chain material |
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