CN1654551A - Method for modifying nano calcium carbonate - Google Patents
Method for modifying nano calcium carbonate Download PDFInfo
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- CN1654551A CN1654551A CN 200510023580 CN200510023580A CN1654551A CN 1654551 A CN1654551 A CN 1654551A CN 200510023580 CN200510023580 CN 200510023580 CN 200510023580 A CN200510023580 A CN 200510023580A CN 1654551 A CN1654551 A CN 1654551A
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- calcium carbonate
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Abstract
The present invention relates to nanometer calcium carbonate modifying process, and is especially the nanometer calcium carbonate emulsion activating process. Binary star surfactant diphosphate is used as the modifier for coating activation treatment of nanometer calcium carbonate emulsion prepared through carbonating process. The preparation process includes the following steps: compounding nanometer calcium carbonate emulsion; controlling the temperature of nanometer calcium carbonate emulsion in 50-100 deg.c and regulating the pH value in 6.0-7.5; adding the said surface modifier via stirring at 50-100 deg.c; controlling reaction time in 15-60 min; filtering the processed nanometer calcium carbonate emulsion to obtain filter cake; and drying the filter cake at 80-130 deg.c, crushing and sieving to obtain active nanometer calcium carbonate product.
Description
Technical field
The present invention relates to a kind of method of modifying of nano-calcium carbonate, is the activation method of nano-calcium carbonate emulsion specifically.
Background technology
Nano-calcium carbonate all is widely used in a lot of fields as a kind of important inorganic materials.One of them important purposes is to be used for Industrial products such as plastics, rubber and coating as filler.Because the own specific surface area of Nano particles of calcium carbonate and specific surface energy is all very high, surface polarity is strong, in the organic medium of nonpolar, low-pole, be not easy to disperse.Therefore, the agglomeration between Nano particles of calcium carbonate is very serious, and is poor with the affinity of organic polymer; These shortcomings greatly reduce its application performance.So, people adopt the whole bag of tricks that nano-calcium carbonate is carried out organic modification of surface, be activation treatment again, to reduce Nano particles of calcium carbonate surface polarity and specific surface energy, thereby the agglomeration between the minimizing Nano particles of calcium carbonate improves the affinity of Nano particles of calcium carbonate and organic polymer and in the intrinsic dispersiveness of organic polymer.
The properties-correcting agent that in the past was used for the nano-calcium carbonate organic modification of surface nearly all is various lipid acid and its esters, resinous acid and its esters.Since the acidity of lipid acid, Resin Acid material a little less than, so lipid acid, resinous acid and its esters must could soluble in waterly well react with the nano-calcium carbonate surface under the higher pH condition.Often alkalescence is stronger for the active nano-calcium carbonate product that makes like this, the pH value usually 9.0, so that more than 9.5.Such active nano-calcium carbonate product can impel plastics such as PVC to decompose adding the man-hour generating unit, thereby significantly reduces the quality product of PVC plastics.
Simultaneously, because lipid acid, Resin Acid material and the solubleness of its esters in water are less, even so (greater than 80 ℃) also are difficult to fully react with the nano-calcium carbonate surface under higher temperature, a large amount of properties-correcting agent are suspended in the nano-calcium carbonate emulsion and form foam, modifying function can not be played, filtering load can be increased on the contrary.So method of modifying properties-correcting agent consumption in the past is big, utilization ratio is low, energy consumption height, troublesome poeration.
Because the bonding force that lipid acid, Resin Acid material, oil substances and nano-calcium carbonate surface form is strong inadequately, therefore often be difficult to guarantee that product has high activation rate, and it is remarkable inadequately to be used for the effect of organic polymer MR medium reinforcing.
Summary of the invention
The object of the present invention is to provide a kind of surface modifying method of nano-calcium carbonate.This method has overcome prior art activation temperature height, and the active nano-calcium carbonate alkalescence of production is strong partially, activation rate and the low shortcoming of surface-modifying agent adsorption rate.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method of modifying of nano-calcium carbonate, it is characterized by and adopt Gemini tensio-active agent bisphosphate salt as properties-correcting agent, the nano-calcium carbonate emulsion that Carbonization Preparation is obtained coats activation treatment, and described Gemini surface-modifying agent bisphosphate (salt) has following molecular structure:
In the following formula:
M is an alkali metal atom;
R
1Be C
4-C
12Alkyl or phenyl or C
4-C
36The assorted carbochain that contains O;
R
2,, R
3Be H atom, perhaps C
8-C
32Alkyl or phenyl or C
8-C
52The assorted carbochain that contains O;
Its method of modifying is as follows:
A. the nano-calcium carbonate that Carbonization Preparation is obtained is made into CaCO
3The quality meter contains the emulsion that the nano-calcium carbonate calcium concn is 5-30%;
B. the temperature of controlling the nano-calcium carbonate emulsion is at 50 ℃-100 ℃, and the pH value of regulating the nano-calcium carbonate emulsion is to 6.0-7.5; Add above-mentioned surface-modifying agent, its add-on is the 0.5-4% of lime carbonate quality; Stir and maintain the temperature in 50 ℃ of-100 ℃ of scopes; Controlling reaction time was at 15-60 minute.
C. will discard filtrate through the nano-calcium carbonate emulsion filtered while hot after the above-mentioned processing, it is dry under 80-130 ℃ to get filter cake, pulverizes, and sieves and promptly gets the active nano-calcium carbonate finished product.
Above-mentioned R
1Be that to have basic structural unit be " O (C
2H
4O) n-" chain forge, number of repeat unit n is 2-18; Described R
2, R
3Have following structure:
Wherein, m is the integer of 2-12, and number of repeat unit n is 2-18.
The inventive method is compared with prior art, have following conspicuous outstanding feature and marked improvement: because the good water solubility of bisphosphate (salt), activation temperature can be low to moderate 50 ℃, and nano-calcium carbonate activation rate height, surface-modifying agent adsorption rate height, the less residue of surface-modifying agent in filtrate is so the amount of used surface-modifying agent significantly is less than original technology among the present invention.Simultaneously, because bisphosphate (salt) can form two chemical bonds (the multiple spot anchor closes) with the nano-calcium carbonate surface, bonding force is strong.It is remarkable to be used for the effect of organic polymer MR medium reinforcing.In addition, Gemini surface-modifying agent bisphosphate (salt) pH value of aqueous solution can be adjusted in about 7.0-8.0 scope, the pH value of the nano-calcium carbonate calcium product after the activated processing is about the 7.0-8.5 scope, like this time as the filler of plastics such as PVC, the active nano-calcium carbonate product impels plastics such as PVC will reduce adding the effect that man-hour, generating unit was decomposed, and will reduce greatly the influence that reduces PVC plastic prod quality.
The preparation method of surface-modifying agent-bisphosphate (salt) that the present invention adopts sees also Chemical physicsletters.303 (1999): 295-303, Sima De, Vinod K.Aswal.
Embodiment
Embodiment one: the skeleton symbol of the surface-modifying agent that is adopted is:
2 kilograms of not surface treated dried nano-calcium carbonates are added water to 9 liters of cumulative volumes, stir into the nano-calcium carbonate emulsion, be heated to 55 ℃ under stirring, use CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, above-mentioned surface-modifying agent 40g is dissolved in 1 liter 55 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot.Discard filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.0-8.0, oil-absorption(number) (DOP) is about 28g/100g CaCO
3This active nano-calcium carbonate is applicable to makes hard PVC plastics and rubber, the filler of coating.
Embodiment two: the skeleton symbol of the surface-modifying agent that is adopted is:
50-60 ℃ of insulation ageing was heated to 65 ℃ after 2 hours to the nano-calcium carbonate emulsion 9 liters (grog contains about 1.4 kilograms of nano-calcium carbonate quality) that Carbonization Preparation is obtained through stirring also, used CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, surface-modifying agent 30g is dissolved in 1 liter 65 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot discards filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.5-8.5, oil-absorption(number) (DOP) is about 26g/100g CaCO
3This active nano-calcium carbonate is applicable to and improves hard PVC plastic working performance, or is used as PP, the filler of HDPE plastics.
The certain applications performance of nano-calcium carbonate after the modification:
1, tensile strength
Table 1 modified nano calcium carbonate is filled the tensile strength (Mpa) of hard PVC material
| ???CaCO 3Add-on wt% | Unmodified | Sodium stearate | Titanic acid ester | Embodiment 1 | Embodiment 2 |
| ????30 ????50 | ????38.4 ????33.3 | ????39.8 ????35.1 | ????40.6 ????35.3 | ????43.7 ????38.0 | ????41.4 ????36.9 |
2, elongation at break:
Table 2 modified nano calcium carbonate is filled the elongation at break (%) of hard PVC material
| ??CaCO 3Add-on wt% | Unmodified | Sodium stearate | Titanic acid ester | Embodiment 1 | Embodiment 2 |
| ????30 ????50 | ????54 ????46 | ????76 ????50 | ????86 ????52 | ????98 ????58 | ????101 ????59 |
3, shock strength
Table 3 modified nano calcium carbonate is filled the notched Izod impact strength (kJ/m of hard PVC material
2)
| CaCO 3Add-on wt% | Unmodified | Sodium stearate | Titanic acid ester | Embodiment 1 | Embodiment 2 |
| ????0 | ????8.7 | ||||
| ????30 ????50 | ??8.9 ??10.1 | ????10.8 ????12.1 | ????11.9 ????13.1 | ????12.3 ????13.6 | ????11.6 ????13.3 |
4, processing characteristics
Table 4 modified nano calcium carbonate is filled the rheological data of hard PVC material
| Test item | Unmodified | Sodium stearate | Titanic acid ester | Embodiment 1 | Embodiment 2 |
| Fusion time (S) plasticization temperature (℃) balancing torque (Nm) | ??314 ??201 ??28.4 | ????305 ????197 ????23.7 | ????301 ????197 ????21.4 | ????295 ????198 ????22.1 | ????266 ????198 ????19.2 |
Embodiment three: the skeleton symbol of the surface-modifying agent that is adopted is:
50-60 ℃ of insulation ageing was heated to 65 ℃ after 2 hours to the nano-calcium carbonate emulsion 9 liters (grog contains about 1.4 kilograms of nano-calcium carbonate quality) that Carbonization Preparation is obtained through stirring also, used CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, surface-modifying agent 30g is dissolved in 1 liter 65 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot discards filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.5-8.5, oil-absorption(number) (DOP) is about 26g/100g CaCO
3This active nano-calcium carbonate is applicable to and improves hard PVC plastic working performance, or is used as PP, the filler of HDPE plastics.
Embodiment four: the skeleton symbol of the surface-modifying agent that is adopted is:
50-60 ℃ of insulation ageing was heated to 70 ℃ after 2 hours to the nano-calcium carbonate emulsion 9 liters (grog contains about 1.4 kilograms of nano-calcium carbonate quality) that Carbonization Preparation is obtained through stirring also, used CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, above-mentioned bisphosphate sodium salt 40g is dissolved in 1 liter 70 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot discards filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.5-8.5, oil-absorption(number) (DOP) is about 24g/100g CaCO
3
This active nano-calcium carbonate has big apparent volume, and product is very fluffy light.
The apparent volume of table 5 modified nano calcium carbonate
Unmodified sodium stearate embodiment 3
48???????????60?????????????76
Embodiment five: the skeleton symbol of the surface-modifying agent that is adopted is:
50-60 ℃ of insulation ageing was heated to 60 ℃ after 2 hours to the nano-calcium carbonate emulsion 9 liters (grog contains about 1.4 kilograms of nano-calcium carbonate quality) that Carbonization Preparation is obtained through stirring also, used CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, above-mentioned bisphosphate sodium salt 35g is dissolved in 1 liter 60 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot discards filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.5-8.5, oil-absorption(number) (DOP) is about 29g/100g CaCO
3
Embodiment six: the skeleton symbol of the surface-modifying agent that is adopted is:
50-60 ℃ of insulation ageing was heated to 60 ℃ after 2 hours to the nano-calcium carbonate emulsion 9 liters (grog contains about 1.4 kilograms of nano-calcium carbonate quality) that Carbonization Preparation is obtained through stirring also, used CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, above-mentioned bisphosphate sodium salt 35g is dissolved in 1 liter 60 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot discards filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.5-8.5, oil-absorption(number) (DOP) is about 29g/100g CaCO
3
Embodiment seven: the skeleton symbol of the surface-modifying agent that is adopted is:
50-60 ℃ of insulation ageing was heated to 60 ℃ after 2 hours to the nano-calcium carbonate emulsion 9 liters (grog contains about 1.4 kilograms of nano-calcium carbonate quality) that Carbonization Preparation is obtained through stirring also, used CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, above-mentioned bisphosphate sodium salt 45g is dissolved in 1 liter 60 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot discards filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.5-8.5, oil-absorption(number) (DOP) is about 30g/100g CaCO
3
The surface-modifying agent of embodiment five and embodiment six has certain wetting ability, and wetting ability is with " (C
2H
4O) n-" in repeating unit n number increase and increase, can between 2-18, regulate according to the needs n number of product performance, n described here is meant the mean number of repeating unit.
Embodiment eight: the skeleton symbol of the surface-modifying agent that is adopted is:
50-60 ℃ of insulation ageing was heated to 60 ℃ after 2 hours to the nano-calcium carbonate emulsion 9 liters (grog contains about 1.4 kilograms of nano-calcium carbonate quality) that Carbonization Preparation is obtained through stirring also, used CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, above-mentioned bisphosphate sodium salt 45g is dissolved in 1 liter 60 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot discards filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.5-8.5, oil-absorption(number) (DOP) is about 30g/100g CaCO
3
The surface-modifying agent of embodiment five and embodiment eight has certain wetting ability, and wetting ability is with " (C
2H
4O) n-" in repeating unit n number increase and increase, can between 2-18, regulate according to the needs n number of product performance, n described here is meant the mean number of repeating unit.
Embodiment nine: the skeleton symbol of the surface-modifying agent that is adopted is:
50-60 ℃ of insulation ageing was heated to 95 ℃ after 2 hours to the nano-calcium carbonate emulsion 9 liters (grog contains about 1.4 kilograms of nano-calcium carbonate quality) that Carbonization Preparation is obtained through stirring also, used CO
2(or Na
2CO
3) regulate the pH value to 6.5-7.0.In addition, above-mentioned bisphosphate sodium salt 35g is dissolved in 1 liter 60 ℃ the hot water and regulates the pH value, again this solution is under agitation added in the above-mentioned nano-calcium carbonate emulsion to 6.5-7.5.Stirring also is incubated 30 minutes.Filtered while hot discards filtrate, get filter cake be cut into strip about 1cm * 1cm * 5cm in baking oven in 120 ℃ dry down, roll pulverizing after the cooling, 160 orders sieve and promptly get the active nano-calcium carbonate finished product.Finished product activation rate 〉=98%, 2% aqeous suspension pH value 7.5-8.5, oil-absorption(number) (DOP) is about 29g/100g CaCO
3
Claims (2)
1. the method for modifying of a nano-calcium carbonate, it is characterized by and adopt Gemini tensio-active agent bisphosphate salt as properties-correcting agent, the nano-calcium carbonate emulsion that Carbonization Preparation is obtained coats activation treatment, and described Gemini surface-modifying agent bisphosphate (salt) has following molecular structure:
In the following formula:
M is an alkali metal atom;
R
1Be C
4-C
12Alkyl or phenyl or C
4-C
36The assorted carbochain that contains O;
R
2,, R
3Be H atom, perhaps C
8-C
32Alkyl or phenyl or C
8-C
52The assorted carbochain that contains O;
Its method of modifying is as follows:
A. the nano-calcium carbonate that Carbonization Preparation is obtained is made into CaCO
3The quality meter contains the emulsion that the nano-calcium carbonate calcium concn is 5-30%;
B. the temperature of controlling the nano-calcium carbonate emulsion is at 50 ℃-100 ℃, and the pH value of regulating the nano-calcium carbonate emulsion is to 6.0-7.5; Add above-mentioned surface-modifying agent, its add-on is the 0.5-4% of lime carbonate quality; Stir and maintain the temperature in 50 ℃ of-100 ℃ of scopes; Controlling reaction time was at 15-60 minute.
C. will discard filtrate through the nano-calcium carbonate emulsion filtered while hot after the above-mentioned processing, it is dry under 80-130 ℃ to get filter cake, pulverizes, and sieves and promptly gets the active nano-calcium carbonate finished product.
2. the method for modifying of nano-calcium carbonate according to claim 1 is characterized in that described R
1Be polyoxyethylene glycol, its basic structural unit is " O-(C
2H
4O) n-", number of repeat unit n is 2-18; Described R
2,, R
3Have following structure:
Wherein, m is the integer of 2-12, and number of repeat unit n is 2-18.
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|---|---|---|---|
| CNB2005100235807A CN100334166C (en) | 2005-01-26 | 2005-01-26 | Method for modifying nano calcium carbonate |
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ID=34894303
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| CN101891909A (en) * | 2010-07-14 | 2010-11-24 | 西南石油大学 | Multifunctional nano CaCO3 reinforced nitrile rubber |
| CN101451023B (en) * | 2007-12-04 | 2012-05-09 | 比亚迪股份有限公司 | Surface modified nano calcium carbonate and polychloroethylene plastisol thereof |
| US9827335B2 (en) | 2009-10-30 | 2017-11-28 | General Electric Company | Treating water insoluble nanoparticles with hydrophilic alpha-hydroxyphosphonic acid conjugates, the so modified nanoparticles and their use as contrast agents |
| CN107987507A (en) * | 2017-12-15 | 2018-05-04 | 上海东大化学有限公司 | The nano-calcium carbonate of polyether carboxylation's modification, include its fluid sealant and preparation method thereof |
| CN108102431A (en) * | 2017-12-15 | 2018-06-01 | 上海东大化学有限公司 | The phosphate-modified nano-calcium carbonate of polyethers includes its fluid sealant and preparation method thereof |
| CN110183876A (en) * | 2019-06-21 | 2019-08-30 | 中国矿业大学(北京) | Powdered whiting modifying agent, the method for modifying of powdered whiting, modified heavy calcium carbonate and its application |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2001508401A (en) * | 1996-06-13 | 2001-06-26 | グレート・レークス・ケミカル・コーポレーション | Method for producing aryl diphosphate esters |
| CN1212273C (en) * | 2001-07-27 | 2005-07-27 | 长春赛纳纳米集团有限公司 | Preparation method of surface modified nano calcium carbonate |
| CN1211286C (en) * | 2001-08-03 | 2005-07-20 | 上海华明高技术（集团）有限公司 | Industrial process for preparing nm-class active calcium carbonate |
| MY142319A (en) * | 2002-08-20 | 2010-11-15 | Malaysian Palm Oil Board Mpob | Extraction of palm vitamin e, phytosterols and squalene from palm oil |
| CN100457632C (en) * | 2002-12-31 | 2009-02-04 | 上海大学 | Method for preparing nano active calcium carbonate |
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2005
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| CN101451023B (en) * | 2007-12-04 | 2012-05-09 | 比亚迪股份有限公司 | Surface modified nano calcium carbonate and polychloroethylene plastisol thereof |
| US9827335B2 (en) | 2009-10-30 | 2017-11-28 | General Electric Company | Treating water insoluble nanoparticles with hydrophilic alpha-hydroxyphosphonic acid conjugates, the so modified nanoparticles and their use as contrast agents |
| CN101891909A (en) * | 2010-07-14 | 2010-11-24 | 西南石油大学 | Multifunctional nano CaCO3 reinforced nitrile rubber |
| CN101891909B (en) * | 2010-07-14 | 2011-11-16 | 西南石油大学 | Multifunctional nano CaCO3 reinforced nitrile rubber |
| CN107987507A (en) * | 2017-12-15 | 2018-05-04 | 上海东大化学有限公司 | The nano-calcium carbonate of polyether carboxylation's modification, include its fluid sealant and preparation method thereof |
| CN108102431A (en) * | 2017-12-15 | 2018-06-01 | 上海东大化学有限公司 | The phosphate-modified nano-calcium carbonate of polyethers includes its fluid sealant and preparation method thereof |
| CN107987507B (en) * | 2017-12-15 | 2020-02-07 | 上海东大化学有限公司 | Polyether carboxylate modified nano calcium carbonate, sealant containing polyether carboxylate modified nano calcium carbonate and preparation method of sealant |
| CN108102431B (en) * | 2017-12-15 | 2020-06-30 | 上海东大化学有限公司 | Polyether phosphate modified nano calcium carbonate, sealant containing polyether phosphate modified nano calcium carbonate and preparation method of sealant |
| CN110183876A (en) * | 2019-06-21 | 2019-08-30 | 中国矿业大学(北京) | Powdered whiting modifying agent, the method for modifying of powdered whiting, modified heavy calcium carbonate and its application |
| CN113416430A (en) * | 2021-06-29 | 2021-09-21 | 常州碳酸钙有限公司 | Preparation method and application of special nano calcium carbonate for polyurethane sealant |
| CN114410129A (en) * | 2022-02-16 | 2022-04-29 | 安徽省宣城市华纳新材料科技有限公司 | Nano calcium carbonate for double-component MS sealant and surface treatment method thereof |
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