CN101967310A - Method for preparing nano calcium carbonate with low viscosity and medium thixotropic property - Google Patents
Method for preparing nano calcium carbonate with low viscosity and medium thixotropic property Download PDFInfo
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- CN101967310A CN101967310A CN 201010226657 CN201010226657A CN101967310A CN 101967310 A CN101967310 A CN 101967310A CN 201010226657 CN201010226657 CN 201010226657 CN 201010226657 A CN201010226657 A CN 201010226657A CN 101967310 A CN101967310 A CN 101967310A
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Abstract
The invention discloses a method for preparing nano calcium carbonate with low viscosity and medium thixotropic property, which comprises the following steps of: calcining and slaking preferred limestone, then controlling carbonization in a membrane reactor to obtain raw nano calcium carbonate slurry, performing composite surface modification treatment on the nano calcium carbonate by using polyester dispersant and fatty acid (or sodium salt), and finally dehydrating, drying, crushing and grading the wrapped slurry. The obtained powder has good dispersion performance, low viscosity and medium thixotropic property, and is suitable for situations with different requirements such as high-performance silicone adhesive, epoxy glue, polysulfide glue, polyurethane glue, automobile prime coat, floor patient and the like. The method has remarkable advantages of easily obtained raw materials, simple process requirement, low production cost and the like, and is easy to control the production process.
Description
Technical field
The invention belongs to the preparing technical field of surface modification treatment nano-calcium carbonate, especially relate to the method that a kind of preparation has low viscosity and medium thixotropic property nano-calcium carbonate, be used for the organic/inorganic composite functional nano-calcium carbonate powder body material of tackiness agent, seal gum and paint field.
Background technology
Lime carbonate (CaCO
3) powder is a kind of important inorganic chemical product, can be widely used in rubber, plastics, Jiao Nianji ﹠amp as powder additives; In the industries such as seal gum, coating and papermaking, play weighting agent usually, promptly increase product volume, reduce cost.Wherein water-ground limestone and common light calcium carbonate are conventional extender filler.Nano grade inorganic particle/polymer composites is a kind of type material with significant application value in the nano material.Can be widely used among rubber, plastics, the fiber three big synthetic materialss.Adopt nano grade inorganic particle preparation polymer matrix composite in modifications such as the reinforcement of material, toughness reinforcing, obstruct, to obtain good effect, also can be used for telomerized polymer fluidic rheological property.The nano grade inorganic particle that can be used for polymer matrix composite at present has many kinds such as nanometer grade calcium carbonate, nanometer grade silica, nano titanium oxide.Wherein, nanometer grade calcium carbonate is because of the ubiquity of its application, cheap price, and characteristic such as nontoxic pollution-free, is widely used in many industries such as rubber, plastics, tackiness agent, papermaking, coating, printing ink, medicine.Therefore, nano-calcium carbonate is from showing the broad applicability of product and the vigorous market requirement once coming out.
The nano-calcium carbonate surface is hydrophilic oleophobic property, easily forms aggregate, bad dispersibility, and directly effect is bad.Therefore, need carry out surface modification treatment, to overcome the defective of powder itself to the nano-calcium carbonate calcium powder.The nano-calcium carbonate calcium powder can make its surface produce performances such as new physics, chemistry, machinery by surface modification, thereby obtains the mineral filler used in purposes more widely such as plastics, rubber, tackiness agent, the coatings industry.The nano-calcium carbonate of surface modification has good strengthening action to the self cure silicone adhesive, can solve ordinary calcium carbonate and cause that system is easily trickled, extrudability poor, defective such as intensity is low, substitutes expensive gas-phase silica in a large number, and practical value is higher.In addition, some investigators are arranged, with nano-calcium carbonate and TiO
2Powder directly mixes being applied in the plastics, found that not only to have replaced the part titanium white, has reduced cost, and has improved the correlated performances such as opacifying power projection ratio of titanium white.This major cause is the character because of the strong interaction on the small scale of nanoparticle and surface, thereby the character of composite bed is fully improved.
Nano-calcium carbonate be used in have good gloss in senior printing ink, the coating, transparent, stable, fast characteristic such as do.In the coatings industry, nano-calcium carbonate not only can be used as the pigment extender that brightens, and increase-volume reduces cost, and improves the gloss of paint of coating, improves glossiness, drying property and the opacifying power of product, also has strengthening action simultaneously.In addition, also be used widely at industry nano-calcium carbonates such as food, medicine, makeup, thereby opened up more wide Application Areas.
Domestic and international in recent years CaCO
3The surface modification treatment technical study very active.The CaCO that surface modification treatment is crossed
3The demand of powder-product constantly increases, abroad at CaCO
3Many treatment processs have been developed in powder surface modification field, surface treatment CaCO
3The powder-product kind is also growing with each passing day.Mainly be engaged in the development of coating calcium carbonate for special use as Britain, its vehicle paint base special surface modified calcium carbonate powder then occupies whole Europe market always.The U.S. then focuses on the research of lime carbonate on papermaking and coating.Though the active CaCO of tens trades mark such as domestic existing " calcene ", " section's power ", " credit China ", " Jia Wei "
3Product lot quantity is produced, but treatment process falls behind mostly, and method is single, and quality product is low, can't with high-grade import CaCO
3Product competition.
In application processes such as tackiness agent, automobile primary coat and terrace lacquer, require sizing material to have good thixotropic property and low viscosity, the active nano-calcium carbonate thixotropy that common surface-modifying agent is handled is relatively poor, even does not have.That more existing researchs have adopted one or several and the lipid acid in titanic acid ester, aluminic acid ester, aluminium titanic acid ester, the silane coupling agent etc. to carry out is composite modified/coat.Other has some researchs to use crystalline form conditioning agents such as nucleus inhibitor, sulfuric acid such as citric acid, and dispersion agents such as dodecyl triethyl amine bromide and some conventional surfactants, in order to improve thixotropy and to reduce viscosity.But these method of modifying effects are not fairly obvious.
CaCO
3Strengthening action and the particle diameter of himself, particle structure and surface chemical property etc. direct relation is arranged.Fill out the development of agent according to benefit, can reduce the particle granular to the requirement of three large attributes, particle structure is complicated, surface activation.With the room temperature vulcanized silicone rubber is example, and this calcium carbonate-filled class system is a pseudoplastic fluid.Reduce with the lime carbonate particle diameter, the viscosity of system increases, and the less system of lime carbonate particle diameter, accelerates with rate of straining, and viscosity degradation is very fast, illustrate the lime carbonate particle diameter than hour, the thixotropy of system is better.But too small particle causes the fast rise of viscosity and surrender, and processing mixing process needs powerful energy input, so that makes machine to run well.In use also there is same problem in product.Thereby take all factors into consideration be used for this class system the nano-calcium carbonate particles size at 50-100nm, by in carbonization process, adding the crystal formation control agent,, help controlling the initial size of nano-calcium carbonate thus as the material of sucrose, this class poly-hydroxy structure of beet sugar.
Discrete particles and external phase liquid mixing form complicated fluid, be common in systems such as tackiness agent, seal gum, coating, plastic melt, rubber melt, the rheological behaviour of studying these systems has important effect to the preparation and the application of these systems, and this variation relation of wherein studying between viscosity and the shearing rate (shear-stress) is main object.Usually so-called " shear shinning " fluid is pseudoplastic fluid.In this case, the viscosity of system has opposite variation tendency with shearing rate, and viscosity reduced when shearing rate increased.The thixotropy that we were concerned about is meant that viscosity not only has relation with shearing force, and with the time relation is arranged also.Pseudoplastic fluid has different viscosity with the variation of shearing rate, but this viscosity is not subjected to time effects.Sheared under the constant shearing rate when a fluid, along with the prolongation of shear time, viscosity can descend gradually.In a single day shearing force is removed, and viscosity will be got back to initial value, but recovery process needs for some time, and this character is called thixotropy.Thixotropic fluid flow and viscograph is one typical " hysteresis loop ", promptly remove the shear shinning curve that viscosity recovery curve after the shearing force begins under the equilibrium state when initial and do not overlap.
Nano-calcium carbonate viscosity, thixotropic property test process:
At first dispose thixotropic fluid, accurately take by weighing quantitative nano-calcium carbonate/calcium oxide/DOP in glass beaker, ratio is CaCO
3: CaO: DOP=100: 10: 175.Above-mentioned system guarantees that at 2000rpm high-speed stirring 5min blending dispersion is even.Then beaker is sealed, be placed in the thermostatic constant wet equipment, require temperature to be controlled at 25 ± 1 ℃, relative humidity is controlled at below 50%.
Treat to use rheometer HAAKE VT 550 tests after above-mentioned thixotropic fluid leaves standstill 24hr.The variation program of shearing rate is during test: in 1 minute by 0s
-1Rise to 452s
-1, kept 5 minutes, in 1 minute, reduce to 0s then
-1
According to the thixotropy of the measured thixotropic loop area judgement nano-calcium carbonate/DOP system of rheometer, the thixotropic loop area is big more, shows that the time dependent degree of viscosity of this system is big more, and just thixotropy is good more.The thixotropic behaviour mechanism of nano-calcium carbonate/DOP system: under the constant temperature static condition, nanometer CaCO
3Between the particle and nanometer CaCO
3Between surface group and the DOP, owing to multiple effects such as hydrogen bond, sterically hindered, electrostatic interaction form stable three-dimensional net structure.Along with the continuous increase of shearing force, hydrogen bond is forced to open one by one, each other the position away from, static and space behavior change, and make that the equilibrium state of above-mentioned network structure is destroyed gradually.After shearing force was removed, because pedesis and aforementioned several effect, system progressively returned to the three-dimensional net structure of equilibrium state, and this recovery process needs the regular hour, so this diagram of system reveals thixotropic behaviour.Shortcomings such as existing surface modification treatment nano-calcium carbonate ubiquity dispersing property is bad, thixotropy is poor, viscosity height, surface treatment agent complicated component, complex process and cost height.
Summary of the invention
The objective of the invention is: at the problem of prior art existence, providing a kind of adopts preparation to have the method for low viscosity and medium thixotropic property nano-calcium carbonate, the treatment process that adopts the composite modified nano-calcium carbonate wet method of polyester dispersion agent and lipid acid (or sodium salt) to coat, the nano-calcium carbonate of handling through this method modification has low viscosity and medium thixotropic property, and has good dispersing property.
Technical scheme of the present invention is: may further comprise the steps successively:
(1), be transferred to kiln after Wingdale cleaned, 800-1200 ℃ of calcining, add water 70-100 ℃ digest 5-15%Ca (OH)
2Slurries.
(2), with Ca (OH)
2Slurries are put into proprietary film and are disperseed carbonization reactor, add one or more the mixture in the carbohydrate crystal formation control agent sucrose, beet sugar, maltose of 0.1-2.5%, feed 15-50% (v) CO
2Controlled temperature carries out carbonization between 5-30 ℃, when the pH value is reduced to 6.5-7.0, continue ventilation 5-10min, obtains the original slurry of nano-calcium carbonate, and three hours apparent settling volumes that guarantee every 100ml slurry are at 85-99ml.
(3), select for use a kind of or more than one mixtures in the longer chain fatty acids such as Palmiticacid, stearic acid, oleic acid, lauric acid as coating, require wherein the fatty acid content of carbonatoms between 18-20 greater than 50%, in the hydrothermal solution of caustic soda, add above-mentioned lipid acid, the caustic soda consumption accounts for the 5-14% of lipid acid, controlled temperature is at 60-80 ℃, reaction 10min-30min, the saponification coating liquid of formation 1-10%; If use the sodium salt of above-mentioned lipid acid then do not need saponification, directly sodium salt is dissolved in the 60-80 ℃ of hot water and obtains saponification liquor; Add the dispersion agent of polyester in above-mentioned saponification liquor, this type of dispersion agent contains multiple functional groups such as hydroxyl, carboxyl, can be anchored at the surface of lime carbonate by functional group.
(4), the specific surface area 20-40m of powder after the preferred drying
2The original slurry of the nano-calcium carbonate of/g.Powerful agitation condition is the original slurry of heating nano-calcium carbonate down, and controlled temperature adds the good adipic acid solution of saponification, insulation reaction 30min-90min at 60-90 ℃.With the slurries filtration drying, finally form surface-treated nano-calcium carbonate powder after the reaction.
Described saponification coating is a longer chain fatty acid, and carbonatoms is between C14-C22, and particularly between C16-C20, requirement C18-C20 content wherein is greater than 50%.The longer chain fatty acid addition accounts for the 0.5-6% of butt nano-calcium carbonate, and the coating consumption accounts for the percentage of nano-calcium carbonate quality, calculates according to following formula: specific surface area numerical value * (0.06～0.16) (%).
Described polyester dispersion agent mainly is made up of the anchoring section and the solvent stages of polarity gene, molecular weight between 3000-10000, good thermal stability, addition is in 0.1-10% (based on the amount of butt nano-calcium carbonate).
Described nanometer CaCO
3Be to adopt proprietary high performance membrane reactor made, median size is at 50-100nm, and particle diameter is controlled, narrow distribution, and crystal formation is a cubes.
Remarkable advantages such as beneficial effect of the present invention: compare with present some surface treatment methods, the present invention has raw material and is easy to get, and processing requirement is simple, and production process is easy to control, and product good dispersion property, production cost are low.Institute's powder dispersity that obtains can be good, has low viscosity, medium thixotropic property, is applicable to the occasion of different needs, such as high performance silicone adhesive, epoxy glue, poly-sulphur glue, polyurethane adhesive, automobile primary coat and terrace lacquer etc., therefore has vast market prospect.The invention enables production technique simple relatively, operation has improved the rheological property of nano-calcium carbonate than being easier to.Technology of the present invention is reasonable, and is with low cost, and product applications is extensive, and market potential is big, and competitive power is strong, has remarkable economical and social benefit, and advanced technology has novelty and novelty.
Description of drawings
Fig. 1 for sample of the present invention when test yield value and kinematic viscosity with the shearing rate function curve diagram.
Embodiment
Embodiment 1:
Be transferred to kiln after Wingdale cleaned, 1000 ℃ of calcinings, add water 80 ℃ digest 10%Ca (OH)
2Slurries; With Ca (OH)
2Slurries are put into proprietary film and are disperseed carbonization reactor, add 1.5% crystal formation control agent, (the v) CO that feeds 30%
2Controlled temperature carries out carbonization at 20 ℃, when the pH value reduces to 6.8, continues ventilation 8min, obtains the original slurry of nano-calcium carbonate, guarantees three hours apparent settling volume 85-99ml of every 100ml slurry.Add saponification in the water of 8% (accounting for lipid acid) caustic soda and 70 ℃ in 3% (accounting for the butt nano-calcium carbonate) lipid acid, reaction 20min forms 6% saponification liquor, adds 2% (accounting for the butt nano-calcium carbonate) polyester dispersion agent in above-mentioned saponification liquor; The specific surface area 20-40m of preferred dry back powder
2The slurry of/g, agitation condition be the original slurry to 80 of heating nano-calcium carbonate ℃ down, adds the good adipic acid solution of saponification, and insulation reaction 60min with the slurries filtration drying, finally forms surface-treated nano-calcium carbonate powder after the reaction.
Embodiment 2:
Be transferred to kiln after Wingdale cleaned, 1200 ℃ of calcinings, add water 100 ℃ digest 15%Ca (OH)
2Slurries; With Ca (OH)
2Slurries are put into proprietary film and are disperseed carbonization reactor, add one or more the mixture in 2.5% carbohydrate crystal formation control agent sucrose, beet sugar, the maltose, (the v) CO that feeds 50%
2Controlled temperature carries out carbonization at 30 ℃, when the pH value reduces to 7.0, continues ventilation 10min, obtains the original slurry of nano-calcium carbonate, and three hours apparent settling volumes that guarantee every 100ml slurry are at 85-99ml.Add saponification in the water of 14% (accounting for lipid acid) caustic soda and 80 ℃ in 6% (accounting for the butt nano-calcium carbonate) lipid acid, reaction 30min forms 1% saponification liquor, adds 0.1% (accounting for the butt nano-calcium carbonate) polyester dispersion agent in above-mentioned saponification liquor; The specific surface area 20-40m of preferred dry back powder
2The slurry of/g, agitation condition be the original slurry to 90 of heating nano-calcium carbonate ℃ down, adds the good adipic acid solution of saponification, and insulation reaction 90min with the slurries filtration drying, finally forms surface-treated nano-calcium carbonate powder after the reaction.
Embodiment 3:
Be transferred to kiln after Wingdale cleaned, 800 ℃ of calcinings, add water 70 ℃ digest 5%Ca (OH)
2Slurries; With Ca (OH)
2Slurries are put into proprietary film and are disperseed carbonization reactor, add 0.1% crystal formation control agent, (the v) CO that feeds 15%
2Controlled temperature carries out carbonization at 5 ℃, when the pH value reduces to 6.5, continues ventilation 5min, obtains the original slurry of nano-calcium carbonate, and three hours apparent settling volumes that guarantee every 100ml slurry are at 85-99ml.Add saponification in the water of 5% (accounting for lipid acid) caustic soda and 60 ℃ in 0.5% (accounting for the butt nano-calcium carbonate) lipid acid, reaction 10min forms 10% saponification liquor, adds 10% (accounting for the butt nano-calcium carbonate) polyester dispersion agent in above-mentioned saponification liquor; The specific surface area 20-40m of preferred dry back powder
2The slurry of/g, agitation condition be the original slurry to 60 of heating nano-calcium carbonate ℃ down, adds the good adipic acid solution of saponification, and insulation reaction 30min with the slurries filtration drying, finally forms surface-treated nano-calcium carbonate powder after the reaction.
For proving that further the present invention has low viscosity and medium thixotropic property, now embodiments of the invention and Comparative Examples contrast are illustrated.
Wingdale is cleaned, obtain lime powder in the high temperature kiln calcining; Add hot water thermophilic digestion lime and get Ca (OH)
2Slurry removes by filter bigger particle; With Ca (OH)
2Slurry is put into proprietary film and is disperseed carbonization reactor, feed carbonic acid gas and carry out carbonization, add 0.1-2.5% crystal control agent (mixtures of one or more in sucrose, beet sugar, the maltose) at carbonization process, carbonization temperature is controlled between 5-30 ℃.The concentration that obtains nano calcium carbonate primary slurry is at 5-20%, and three hours apparent settled volumes that guarantee every 100ml magma are at 85-99ml.Following if no special instructions each example all adopts above-mentioned carbonization process.
Embodiment 4:
The nano-calcium carbonate slurry of heating 12% is warming up to 75 ℃, stirs 1hr.Meanwhile take by weighing 3.5% lipid acid of (with respect to the butt nano-calcium carbonate, down with) and 10% caustic soda (with respect to the amount of lipid acid, down with), 80 ℃ of following saponification 10min form 5% saponification liquor, add 0.3% polyester dispersion agent simultaneously.Saponification liquor is transferred in the slurry whip modified 60min.And after-filtration, washing, drying, grinding pack.
Embodiment 5:
The nano-calcium carbonate slurry of heating 12% is warming up to 75 ℃, stirs 1hr.Meanwhile take by weighing 1.8% lipid acid and 10% caustic soda, 80 ℃ of following saponification 10min form 5% saponification liquor, add 2% polyester dispersion agent simultaneously.Saponification liquor is transferred in the slurry whip modified 60min.And after-filtration, washing, drying, grinding pack.
Embodiment 6:
The nano-calcium carbonate slurry of heating 12% is warming up to 75 ℃, stirs 1hr.Meanwhile take by weighing 0.8% lipid acid and 10% caustic soda, 80 ℃ of following saponification 10min form 5% saponification liquor, add 3% polyester dispersion agent simultaneously.Saponification liquor is added drop-wise in the slurry continuously whip modified 30min.And after-filtration, washing, drying, grinding pack.
Comparative Examples 1:
The nano-calcium carbonate slurry of heating 12% is warming up to 75 ℃, stirs 1hr.Meanwhile take by weighing 3.8% lipid acid and 10% caustic soda, 80 ℃ of following saponification 10min form 5% saponification liquor.Saponification liquor is transferred in the slurry whip modified 30min.And after-filtration, washing, drying, grinding pack.
Comparative Examples 2:
The nano-calcium carbonate slurry of heating 12% is warming up to 75 ℃, stirs lhr.Meanwhile take by weighing 3.8% lipid acid and 10% caustic soda, 80 ℃ of following saponification 10min form 5% saponification liquor.Saponification liquor is transferred in the slurry whip modified 60min.And after-filtration, washing, drying, grinding pack.
Blank sample: without the nano-calcium carbonate of surface modification treatment.
Above-mentioned case thixotropy result contrasts as follows:
Have low viscosity and medium thixotropic property nano-calcium carbonate example and Comparative Examples as can be seen by above-mentioned enforcement preparation, the present invention adopts polyester dispersion agent and the composite modified nano-calcium carbonate with low viscosity and medium thixotropic property of preparing of lipid acid (or sodium salt).
From sample of the present invention shown in Figure 1 when test yield value and kinematic viscosity with the shearing rate function curve diagram as can be seen, sample yield value when testing by the present invention's preparation is function curve A variation with shearing rate, and kinematic viscosity is function curve B variation with shearing rate, has the characteristics of low viscosity and medium thixotropic property nano-calcium carbonate thereby embody preparation.
Compare with more present surface treatment methods, product viscosity of the present invention reduces, and thixotropic property is medium, have raw material and be easy to get, technological requirement is simple, and production process is easy to control, the remarkable advantage such as product good dispersion property, production cost are low can be used for the fields such as adhesive, fluid sealant and coating.
Claims (7)
1. one kind prepares the method with low viscosity and medium thixotropic property nano-calcium carbonate, it is characterized in that: in turn include the following steps:
(1) be transferred to kiln after Wingdale is cleaned, 800-1200 ℃ of calcining, add water 70-100 ℃ digest 5-15%Ca (OH)
2Slurries;
(2) with Ca (OH)
2Slurries are put into proprietary film and are disperseed carbonization reactor, add one or more the mixture in the carbohydrate crystal formation control agent sucrose, beet sugar, maltose of 0.1-2.5%, feed 15-50% (v) CO
2Controlled temperature carries out carbonization between 5-30 ℃, when the pH value is reduced to 6.5-7.0, continue ventilation 5-10min;
(3) the longer chain fatty acid addition accounts for the 0.5-6% of butt nano-calcium carbonate, the addition of polyester dispersion agent accounts for the 0.1-10% of butt nano-calcium carbonate, in lipid acid, add saponification in the water of 5-14% caustic soda (based on the amount of lipid acid) and 60-80 ℃, reaction 10min-30min, form the saponification coating liquid of 1-10%, if use the sodium salt of above-mentioned lipid acid then do not need saponification, directly sodium salt is dissolved in the 60-80 ℃ of hot water and obtains saponification liquor, in above-mentioned saponification liquor, add the polyester dispersion agent;
(4) the nano-calcium carbonate slurry guarantee every 100ml magma three hours apparent settling volumes at 85-99ml, the specific surface area 20-40m of preferred dry back powder
2The slurry of/g, the agitation condition original slurry of heating nano-calcium carbonate down add the good adipic acid solution of saponification to 60-90 ℃, and insulation reaction 30min-90min with the slurries filtration drying, finally forms surface-treated nano-calcium carbonate powder after the reaction.
2. a kind of preparation according to claim 1 has the method for low viscosity and medium thixotropic property nano-calcium carbonate, it is characterized in that: the high-quality of using, longer chain fatty acid, to between the C22, wherein C18-C20 content is greater than 50%, or the sodium salt of above-mentioned lipid acid at C14 for carbonatoms.
3. a kind of preparation according to claim 2 has the method for low viscosity and medium thixotropic property nano-calcium carbonate, it is characterized in that: selected lipid acid is that a kind of or more than one mixtures in Palmiticacid, stearic acid, oleic acid, the lauric acid etc. are as coating.
4. a kind of preparation according to claim 1 has the method for low viscosity and medium thixotropic property nano-calcium carbonate, it is characterized in that: employed lipid acid consumption accounts for the percentage of nano-calcium carbonate quality, calculates according to following formula:
Specific surface area numerical value * (0.06～0.16) (%).
5. a kind of preparation according to claim 1 has the method for low viscosity and medium thixotropic property nano-calcium carbonate, it is characterized in that: described polyester dispersion agent mainly is made up of anchoring section and solvent chain, anchoring section mainly is the polarity gene that contains multiple functional groups such as hydroxyl, carboxyl, solvent chain mainly is nonpolar long-chain fat carbochain, and molecular weight is between 3000-10000.
6. a kind of preparation according to claim 1 has the method for low viscosity and medium thixotropic property nano-calcium carbonate, it is characterized in that: the preferred 0.5-5% of the addition of described polyester dispersion agent (based on the amount of butt nano-calcium carbonate).
7. a kind of preparation according to claim 6 has the method for low viscosity and medium thixotropic property nano-calcium carbonate, it is characterized in that: the addition of described polyester dispersion agent is 1-3% (based on the amount of butt nano-calcium carbonate) more preferably.
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| CN102167915A (en) * | 2011-03-03 | 2011-08-31 | 淄博嘉泽纳米材料有限公司 | Preparation method of medium/low-viscosity high-thixotropy nano calcium carbonate for aqueous system |
| CN103509378A (en) * | 2013-10-22 | 2014-01-15 | 山西兰花华明纳米材料有限公司 | Normal-temperature high-air-flow industrial nano-calcium carbonate preparation method |
| CN103693669A (en) * | 2013-12-03 | 2014-04-02 | 恩平市嘉维化工实业有限公司 | Method for preparing nano calcium carbonate special for rolling film |
| CN103897434B (en) * | 2014-04-19 | 2016-03-30 | 芮城新泰纳米材料有限公司 | The preparation method that plastic master batch is Nano calcium carbonate dedicated |
| CN105482500A (en) * | 2015-11-25 | 2016-04-13 | 广西华纳新材料科技有限公司 | Surface modification method of anti-oxidation nanometer calcium carbonate used for silicone sealant |
| CN105802280A (en) * | 2016-05-20 | 2016-07-27 | 山西新泰恒信纳米材料有限公司 | Preparation method for nano calcium carbonate (CaCO3) for lubricating grease |
| CN107312361A (en) * | 2017-07-01 | 2017-11-03 | 江西九峰纳米钙有限公司 | A kind of preparation technology for improving nano-calcium carbonate activation rate |
| CN109504130A (en) * | 2018-12-19 | 2019-03-22 | 安徽省宣城市华纳新材料科技有限公司 | A kind of preparation of silane end capped polyurethane sealant nanometer calcium carbonate |
| CN109971216A (en) * | 2019-03-26 | 2019-07-05 | 长沙理工大学 | A kind of preparation method that polyethylene antifog film is Nano calcium carbonate dedicated |
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| 《湖北工业大学学报》 20050428 严海彪等 聚酯超分散剂改性纳米碳酸钙及其应用研究 15-17、24 1-7 第20卷, 第2期 2 * |
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| CN102167915B (en) * | 2011-03-03 | 2013-04-17 | 淄博嘉泽纳米材料有限公司 | Preparation method of medium/low-viscosity high-thixotropy nano calcium carbonate for aqueous system |
| CN103509378A (en) * | 2013-10-22 | 2014-01-15 | 山西兰花华明纳米材料有限公司 | Normal-temperature high-air-flow industrial nano-calcium carbonate preparation method |
| CN103693669A (en) * | 2013-12-03 | 2014-04-02 | 恩平市嘉维化工实业有限公司 | Method for preparing nano calcium carbonate special for rolling film |
| CN103897434B (en) * | 2014-04-19 | 2016-03-30 | 芮城新泰纳米材料有限公司 | The preparation method that plastic master batch is Nano calcium carbonate dedicated |
| CN105482500A (en) * | 2015-11-25 | 2016-04-13 | 广西华纳新材料科技有限公司 | Surface modification method of anti-oxidation nanometer calcium carbonate used for silicone sealant |
| CN105482500B (en) * | 2015-11-25 | 2018-09-14 | 广西华纳新材料科技有限公司 | The surface modifying method of silicone sealant antioxidant nano-calcium carbonate |
| CN105802280A (en) * | 2016-05-20 | 2016-07-27 | 山西新泰恒信纳米材料有限公司 | Preparation method for nano calcium carbonate (CaCO3) for lubricating grease |
| CN107312361A (en) * | 2017-07-01 | 2017-11-03 | 江西九峰纳米钙有限公司 | A kind of preparation technology for improving nano-calcium carbonate activation rate |
| CN109504130A (en) * | 2018-12-19 | 2019-03-22 | 安徽省宣城市华纳新材料科技有限公司 | A kind of preparation of silane end capped polyurethane sealant nanometer calcium carbonate |
| CN109504130B (en) * | 2018-12-19 | 2021-02-09 | 安徽省宣城市华纳新材料科技有限公司 | Preparation of nano calcium carbonate for silane-terminated polyurethane sealant |
| CN109971216A (en) * | 2019-03-26 | 2019-07-05 | 长沙理工大学 | A kind of preparation method that polyethylene antifog film is Nano calcium carbonate dedicated |
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