CN106830043B - A kind of method of surface modified nano calcium carbonate - Google Patents

A kind of method of surface modified nano calcium carbonate Download PDF

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CN106830043B
CN106830043B CN201710223694.9A CN201710223694A CN106830043B CN 106830043 B CN106830043 B CN 106830043B CN 201710223694 A CN201710223694 A CN 201710223694A CN 106830043 B CN106830043 B CN 106830043B
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calcium carbonate
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slurries
surface modified
coupling agent
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CN106830043A (en
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张剑星
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions

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Abstract

A kind of method of surface modified nano calcium carbonate, by quick lime, ashing, iron removaling, digestion, add chemical additives carbonization, obtain nano-calcium carbonate slurries, it is modifying agent by aluminate coupling agent, silane, laurate, nonionic surface active agent compounding, adds in nano-calcium carbonate concentrated slurry, obtain surface modified nano calcium carbonate slurry.This method need not be carried out repeatedly to nano-calcium carbonate, substep surface is modified, activation, the activation rate of obtained surface modified nano calcium carbonate can reach more than 99%, the Effective Regulation particle diameter distribution and activity of product.Coupling agent drastically increases the compatibility between nano-calcium carbonate and organic polymer, improves the rheological property of system.

Description

A kind of method of surface modified nano calcium carbonate
Technical field
The present invention relates to a kind of preparation method of calcium carbonate, particularly a kind of method of surface modified nano calcium carbonate.
Background technology
Nano-calcium carbonate is widely used in rubber industry, plastics industry, paper industry, coatings industry, medical industry etc..Answering With in engineering, nano-calcium carbonate is required to be well dispersed in organic media, so that target material has homogeneous property, However, because the characteristic of nano-calcium carbonate itself causes nano-calcium carbonate to have the problem of certain in application aspect, for example, a side Face, nano grain surface can be high, in thermodynamics unsteady state, are easy to reunite；On the other hand, calcium carbonate system common at present The calcium carbonate surface that Preparation Method obtains is in hydrophily more, is difficult to reach dispersed effect when disperseing in organic media, with Adhesion is low between polymer, results in boundary defect, influences polymer performance.Therefore, people for improve nano-powder with The compatibility of medium interface and the dispersiveness of powder have carried out substantial amounts of trial and effort.At present, for nano-calcium carbonate Surface, which is modified, is broadly divided into dry method modification and wet-process modified.Wherein the modifying agent of dry method modification mainly include titanate esters, Aluminate, Phosphate etc., wet-process modified modifying agent mainly include stearic acid and its salt etc..Although titanate esters modified effect is good, its meeting The whiteness of product is influenceed, price is high and may cause liver cancer, therefore, is abandoned gradually.Aluminate can be in calcium carbonate surface shape Into chemical bond, performance is better than titanate esters, has been widely used, be still, the shortcomings that Aluminate it is susceptible to hydrolysis, therefore, Application for Aluminate is limited to dry method modification, cannot be guaranteed in wet-process modified middle effect.
The content of the invention
The technical problem to be solved in the present invention is to overcome wet-process modified nano-calcium carbonate process to be difficult to apply Aluminate or effect The problem of fruit is bad, there is provided a kind of method for preparing nano-calcium carbonate, and it is wet-process modified using Aluminate progress.
To solve the technical problem of the present invention, used technical scheme is：
A kind of method of surface modified nano calcium carbonate, comprises the following steps：
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, and it is 12- to be carbonized to pH value 13, nano-calcium carbonate slurries are obtained,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）It is modifying agent by aluminate coupling agent, silane, laurate, nonionic surface active agent compounding, by compounding Modifying agent is dissolved in the in the mixed solvent of water and ethanol, standby；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified, the time is 20-30 minutes, is obtained Surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Further, the dosage of the aluminate coupling agent is the 0.5-0.7% of nano-calcium carbonate sodium quality.
Further, aluminate coupling agent, silane, laurate, nonionic surface active agent mol ratio are：1:0.1- 0.3:0.2-0.3:0.3-0.6。
Further, modification is carried out at 50-60 DEG C.
Further, step 5）Reclaimed water and the volume ratio of ethanol are 1:3-7.
Further, the carburizing temperature is 20-30 DEG C.
Further, by step 4）Nano-calcium carbonate slurries after concentration carry out secondary carbonization, then carry out surface and be modified work Change.
Beneficial effect：
Instant invention overcomes can not apply Aluminate in wet-process modified, or dosage is big, ineffective during application Aluminate Defect, the hydrolysis of aluminate coupling agent is suppressed by silane, laurate, nonionic surface active agent, and optimize four Proportioning and dosage, only with the once modified modification that can reach to nano-calcium carbonate surface, activation, it is not necessary to nano-calcium carbonate Calcium is carried out repeatedly, substep surface is modified, activation, and the activation rate that the present invention obtains surface modified nano calcium carbonate can reach 99% More than, the Effective Regulation particle diameter distribution and activity of product.Coupling agent drastically increases nano-calcium carbonate and organic polymer Between compatibility, improve the rheological property of system.
Embodiment
A kind of method of surface modified nano calcium carbonate, comprises the following steps：
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, and it is 12- to be carbonized to pH value 13, nano-calcium carbonate slurries are obtained,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）It is modifying agent by aluminate coupling agent, silane, laurate, nonionic surface active agent compounding, by compounding Modifying agent is dissolved in the in the mixed solvent of water and ethanol, standby；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified, the time is 20-30 minutes, is obtained Surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Further, the dosage of the aluminate coupling agent is the 0.5-0.7% of nano-calcium carbonate quality.
Further, aluminate coupling agent, silane, laurate, nonionic surface active agent mol ratio are：1:0.1- 0.3:0.2-0.3:0.3-0.6。
Further, modification is carried out at 50-60 DEG C
Further, step 5）Reclaimed water and the volume ratio of ethanol are 1:3-7.
Further, the carburizing temperature is 20-30 DEG C.
Further, by step 4）Nano-calcium carbonate slurries after concentration carry out secondary carbonization, then carry out surface and be modified work Change.
Embodiment 1
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.3:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 2
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.6% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.3:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 3
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.7% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.3:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 4
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.8% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.3:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 5
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.4% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.3:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 6
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.05: 0.3:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 7
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.4: 0.3:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 8
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.1:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 9
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.4:0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 10
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.3:0.2；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 11
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, alkylphenol-polyethenoxy Ether compounding is modifying agent, and the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the body of water and ethanol Product is than being 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, bay Acid, nonionic surface active agent mol ratio are：1:0.2: 0.3:0.7；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 12
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）It is modifying agent by aluminate coupling agent, laurate, APES compounding, the modifying agent of compounding is molten It is standby in the in the mixed solvent of water and ethanol；Wherein, the volume ratio of water and ethanol is 1:3-7, the dosage of aluminate coupling agent are The 0.5% of nano-calcium carbonate quality, aluminate coupling agent, laurate, nonionic surface active agent mol ratio are：1: 0.3: 0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 13
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, APES compounding For modifying agent, the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, it is standby；Wherein, the volume ratio of water and ethanol is 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, laurate, it is non-from Subtype surfactant molar ratio is：1:0.2: 0.4；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 14
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）It is modifying agent by aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate compounding, will The modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, standby；Wherein, the volume ratio of water and ethanol is 1:3-7, Aluminate The dosage of coupling agent is the 0.5% of nano-calcium carbonate quality, aluminate coupling agent, silane, laurate, non-ionic surfactant Agent mol ratio is：1:0.2: 0.3；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
Embodiment 15
1）Weigh low-grade quick lime, ashing, iron removaling；
2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieving, filter slurries Ageing；
3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, 20-30 DEG C of carbonization to pH It is worth for 13, obtains nano-calcium carbonate slurries,
4）By step 3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
5）It is modifying agent by aluminate coupling agent, the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, it is standby； Wherein, the volume ratio of water and ethanol is 1:3-7, the dosage of aluminate coupling agent are the 0.5% of nano-calcium carbonate quality；
6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified at 50-60 DEG C, time 20- 30 minutes, obtain surface modified nano calcium carbonate slurry；
7）By step 6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate Powder.
The surface modified nano calcium carbonate activation rate of table 1
Aluminate coupling agent in embodiment 1-15, silane, laurate, nonionic surface active agent dosage, proportioning and Gained surface modified nano calcium carbonate activation rate is referring to table 1.

Claims (5)

  1. A kind of 1. method of surface modified nano calcium carbonate, it is characterised in that：Comprise the following steps：
    （1）Weigh low-grade quick lime, ashing, iron removaling；
    （2）Add in digestion reactor filled with hot water, stir, carry out digestion reaction, stand cooling, sieve, filtering slurries are old Change；
    （3）It is passed through carbon dioxide in slurries to be carbonized, carbonisation adds chemical additives, and it is 12-13 to be carbonized to pH value, is obtained To nano-calcium carbonate slurries,
    （4）By step（3）Obtained nano-calcium carbonate slurries ageing, sedimentation concentration；
    （5）By aluminate coupling agent, aminoethyl aminoethylaminopropyl trimethoxy silane, laurate, APES Compound as modifying agent, the modifying agent of compounding is dissolved in the in the mixed solvent of water and ethanol, it is standby；
    （6）Modifier solution is added in nano-calcium carbonate concentrated slurry, is modified, the time is 20-30 minutes, obtains table Face modified nano calcium carbonate slurry；
    （7）By step（6）Obtained surface modified nano calcium carbonate slurry drying, you can obtain surface modified nano calcium carbonate powder Body；
    The quality of aluminate coupling agent is the 0.5-0.7% of nano-calcium carbonate quality；
    Aluminate coupling agent, silane, laurate, APES mol ratio are：1:（0.1-0.3）:（0.2-0.3）: （0.3-0.6）.
  2. 2. the method as described in claim 1, it is characterised in that：Modification is carried out at 50-60 DEG C.
  3. 3. the method described in claim 1, it is characterised in that：Step（5）Reclaimed water and the volume ratio of ethanol are 1:（3-7）.
  4. 4. the method as described in claim 1, it is characterised in that：The carburizing temperature is 20-30 DEG C.
  5. 5. the method as described in claim 1, it is characterised in that：By step（4）Nano-calcium carbonate slurries after concentration carry out two Secondary carbonization, then carry out surface modified active.
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CN107324368A (en) * 2017-08-10 2017-11-07 青阳县永诚钙业有限责任公司 A kind of preparation method of nano-calcium carbonate
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CN110229542A (en) * 2019-07-22 2019-09-13 恩平燕怡新材料有限公司 A kind of PVC pipe nm-class active calcium carbonate and preparation method thereof, PVC pipe
CN112480713A (en) * 2020-11-27 2021-03-12 安徽省宣城市华纳新材料科技有限公司 Preparation method of nano calcium carbonate for filling polyethylene transparent film
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