CN106675109A - Preparation method of high-activity nano calcium carbonate subjected to surface bioactive treatment - Google Patents
Preparation method of high-activity nano calcium carbonate subjected to surface bioactive treatment Download PDFInfo
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- CN106675109A CN106675109A CN201610993301.8A CN201610993301A CN106675109A CN 106675109 A CN106675109 A CN 106675109A CN 201610993301 A CN201610993301 A CN 201610993301A CN 106675109 A CN106675109 A CN 106675109A
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- calcium carbonate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
Abstract
The invention discloses a preparation method of high-activity nano calcium carbonate subjected to surface bioactive treatment. The method comprises the steps of firstly utilizing wet process surface treatment, carrying out dry process surface treatment and obtaining a high-activity nano calcium carbonate product by using two surface treatment methods. The wet process surface treatment is mainly used for solving the aggregation problem of nano calcium carbonate particles through depolymerizing dispersion in a solution state and carrying out surface treatment when the particles are reduced into the original state. The dry process surface treatment is used for carrying out surface treatment by selecting different surfactants according to the performance characteristics of the designed nano calcium carbonate product model.
Description
Technical field
The present invention relates to a kind of technical field of nano-calcium carbonate manufacture, more particularly to a kind of height work of surface-active-treatment
The preparation method of property nano-calcium carbonate.
Background technology
At present, because nano-calcium carbonate granularity is little, with great specific surface area and higher specific surface energy, easily occur
Particle aggregation makes particle diameter become big, and the function that nanoparticle has is affected when finally using.Meanwhile, calcium carbonate has certain alkali
Property and be in polarity, it is poor with the compatibility of organic polymer, disperse uneven in polymer matrix, cause the mechanical property of material
Decline.Surface modification effect seems particularly significant to nano-calcium carbonate application.The surface modifying method of calcium carbonate can be divided into dry method
Surface treatment and wet process surface treatment.Dry method is primarily now surface-treated using various coupling agents to calcium carbonate powder；It is wet
Method has good coated effect, mainly adopts stearic acid (salt) at present, and so far still among continuous research and development.
The content of the invention
The invention aims to overcome the shortcoming of above-mentioned prior art, there is provided a kind of high activity of surface-active-treatment
The preparation method of nano-calcium carbonate, the preparation method of the high-activity nano calcium carbonate of the surface-active-treatment can significantly improve particle
Dispersiveness and lipophile, activation rate is higher by much than common active calcium carbonate calcium, and oil factor is also low than common active calcium carbonate,
Belong to the preferable nano-calcium carbonate of activity degree.The preparation method adopts two kinds of surface treatment methods of wet method and dry method simultaneously, and solely
Invasively the characteristic of root Ju difference aliphatic acid, adjusts the ratio of fatty acid mixed, characteristic the characteristics of reach deisgn product so that generate
Active nano-calcium carbonate products application when different high polymers, the characteristics of can significantly more show its functional material.
The present invention is mainly first with wet process surface treatment, then carries out dry surface process, using two kinds of surface treatment sides
Method obtains the nano-calcium carbonate calcium product of high activity degree.Wet process surface treatment：Depolymerization dispersion, mainly solves nanometer under solution state
The agglomeration traits of calcium carbonate particle, carry out surface and are modified during the state of particle reduction to most original.Dry surface process：Root Ju
Designed nano-calcium carbonate product type, the performance characteristics having carry out surface and are modified from different surfactants.
The technical solution adopted for the present invention to solve the technical problems is：A kind of high-activity nano carbon of surface-active-treatment
The preparation method of sour calcium, comprises the following steps：
（1）Nano-calcium carbonate emulsion dilutes：The nano-calcium carbonate emulsion generated by carburizing reagent, adds hot water dilution；
（2）It is prepared by neat soap solution：Neat soap proportioning hot water stirs dissolving obtains neat soap solution for standby, and fat is added during stirring and dissolving
Class activating agent accelerates the dissolving of neat soap；
（3）It is prepared by soap emulsion：Laurate, myristic acid, palmitic acid, stearic acid, oleic acid are selected, each aliphatic acid is adjusted
Ratio and characteristic the characteristics of be mixed to form fatty acid mixed to reach deisgn product, after fatty acid mixed proportioning hot water dissolving, plus
Enter sodium hydroxide solution, stir saponification, generate soap emulsion standby；
（4）Wet process surface treatment：First with neat soap solution the nano-calcium carbonate particles after dilution are carried out with Dispersion on surface and is modified, then
Carry out surface with the soap emulsion for making to be modified；
（5）Press filtration；
（6）It is dried and once crushes and forms calcium carbonate particle；
（7）Dry surface process：Coconut oil, palm oil, soybean oil, mineral oil, single stearic acid glycerine lipoprotein, oleamide is selected to make
For surface conditioning agent, calcium carbonate particle surface is processed, the ratio for adjusting each surface conditioning agent reaches the spy of deisgn product
Dot characteristics；
（8）Separating twice, classification are processed and packed, and obtain highly active nano-calcium carbonate.
The step（1）Solution temperature is 50 DEG C~60 DEG C after the dilution of middle nano-calcium carbonate emulsion, solution concentration is 8.0%~
10.0%。
The step（2）Prepared by middle neat soap solution, the neat soap solution temperature after hot water dissolving is 80 DEG C~100 DEG C, after dissolving
Neat soap solution solution concentration be 10.0%~15.0%, lipid activating agent is 10%~50% coconut oil.
The step（3）Prepared by middle soap emulsion, temperature is 80 DEG C~100 after fatty acid mixed proportioning hot water dissolving
DEG C, the solution concentration of soap emulsion is 20.0%~25.0%, and concentration of sodium hydroxide solution is 30%~35%.
The step（4）Middle wet process surface treatment process temperature is controlled between 40-80 DEG C, and surface conditioning agent quality is carbonic acid
The 2.0%~5.0% of calcareous amount.
The step（7）Between 80-110 DEG C, surface conditioning agent quality is the temperature control of middle dry surface processing procedure
The 0.4%~2.0% of calcium carbonate quality.
In sum, the preparation method of the high-activity nano calcium carbonate of surface-active-treatment of the invention can significantly improve grain
The dispersiveness of son and lipophile, activation rate is higher by much than common active calcium carbonate calcium, and oil factor also compares common active calcium carbonate
It is low, belong to the preferable nano-calcium carbonate of activity degree.The preparation method adopts two kinds of surface treatment methods of wet method and dry method simultaneously, and
Originally the characteristic of root Ju difference aliphatic acid, adjusts the ratio of fatty acid mixed, characteristic the characteristics of reach deisgn product so that raw
Into active nano-calcium carbonate products application when the different high polymers, the characteristics of can significantly more show its functional material.
Specific embodiment
Embodiment 1
A kind of preparation method of the high-activity nano calcium carbonate of the surface-active-treatment described by the present embodiment 1, including following step
Suddenly：
Calcium carbonate emulsion and 80 DEG C of hot water are added in the closed storage tank with stirring of 35M3, about 50 DEG C of 10% concentration is adjusted to
The M3 of calcium carbonate soln 30.
90 DEG C of hot water 260kg is added in the closed storage tank with stirring of 1M3, in stirring（200 revs/min）It is lower to add
Enter the neat soap and 9kg coconut oil of 20kg.Continue to stir and make neat soap solution for standby in 50 minutes.
The NaOH of 9.1kg is dissolved in the water of about 25 DEG C of 17kg under stirring, makes the NaOH aqueous solution standby.
In the stirred autoclave of 1.5M3,90 DEG C of hot water 200kg is added, start stirring（200 revs/min）Add
The palmitic acid and 4kg laurate of 49.2kg, after stirring dissolving in 5 minutes, is slowly added to the NaOH aqueous solution got ready.Sealing reaction
Kettle, with steam 130 DEG C are warming up to, and it is standby that mixing time makes soap emulsion up to after 50 minutes.
First the neat soap solution got ready is added in calcium carbonate soln, under 500 revs/min, is stirred 20 minutes.To get ready again
Soap emulsion add calcium carbonate soln in, continue 30 minutes.
Finely dispersed calcium carbonate is obtained after the good calcium carbonate soln press filtration of wet process surface treatment, drying, one-level are crushed
Powder.
By the broken oleamide for being warming up to 100 DEG C, adding 13kg coconut oil and 1kg of above-mentioned nano-powder Jing second patent flours, powder
After broken 10 minutes, after these particle classifyings are processed the preferable nano-calcium carbonate of activity degree is just obtained.
The testing result of resulting powder is shown in Table one：
Embodiment 2
A kind of preparation method of the high-activity nano calcium carbonate of the surface-active-treatment described by the present embodiment 2, including following step
Suddenly：
Calcium carbonate emulsion and 80 DEG C of hot water are added in the closed storage tank with stirring of 35M3, about 50 DEG C of 10% concentration is adjusted to
The M3 of calcium carbonate soln 30.
90 DEG C of hot water 480kg is added in the closed storage tank with stirring of 1M3, in stirring（200 revs/min）It is lower to add
Enter the neat soap and 4kg palm oils of 50kg.Continue to stir and make neat soap solution for standby in 50 minutes.
The NaOH of 7.9kg is dissolved in the water of about 25 DEG C of 15kg under stirring, makes the NaOH aqueous solution standby.
In the stirred autoclave of 1.5M3,90 DEG C of hot water 185kg is added, start stirring（200 revs/min）Add
The palmitic acid of 40kg, 2.3kg laurate, 2.3kg stearic acid and 2.3kg oleic acid, after stirring dissolving in 5 minutes, are slowly added to get ready
The NaOH aqueous solution.Sealed reactor, with steam 130 DEG C are warming up to, and mixing time makes soap emulsion up to after 50 minutes
It is standby.
First the neat soap solution got ready is added in calcium carbonate soln, under 500 revs/min, is stirred 20 minutes.To get ready again
Soap emulsion add calcium carbonate soln in, continue 30 minutes.
Finely dispersed calcium carbonate is obtained after the good calcium carbonate soln press filtration of wet process surface treatment, drying, one-level are crushed
Powder.
100 DEG C are warming up to by above-mentioned nano-powder Jing second patent flours are broken, 16kg palm oils are added, after crushing 10 minutes, by this
A little particle classifyings just obtain the preferable nano-calcium carbonate of activity degree after processing.
The testing result of resulting powder is shown in Table two：
The above, is only presently preferred embodiments of the present invention, not makees any pro forma to technical scheme
Limit.Any simple modification, equivalent variations and modification that every technical spirit according to the present invention is made to above example,
Still fall within the range of technical scheme.
Claims (6)
1. the preparation method of the high-activity nano calcium carbonate of a kind of surface-active-treatment, it is characterised in that comprise the following steps：
（1）Nano-calcium carbonate emulsion dilutes：The nano-calcium carbonate emulsion generated by carburizing reagent, adds hot water dilution；
（2）It is prepared by neat soap solution：Neat soap proportioning hot water stirs dissolving obtains neat soap solution for standby, and fat is added during stirring and dissolving
Class activating agent accelerates the dissolving of neat soap；
（3）It is prepared by soap emulsion：Laurate, myristic acid, palmitic acid, stearic acid, oleic acid are selected, each aliphatic acid is adjusted
Ratio is simultaneously mixed to form fatty acid mixed, after fatty acid mixed proportioning hot water dissolving, adds sodium hydroxide solution, and stirring saponification is anti-
Should, generate soap emulsion standby；
（4）Wet process surface treatment：First with neat soap solution the nano-calcium carbonate particles after dilution are carried out with Dispersion on surface and is modified, then
Carry out surface with the soap emulsion for making to be modified；
（5）Press filtration；
（6）It is dried and once crushes and forms calcium carbonate particle；
（7）Dry surface process：Coconut oil, palm oil, soybean oil, mineral oil, single stearic acid glycerine lipoprotein, oleamide is selected to make
For surface conditioning agent, calcium carbonate particle surface is processed, adjust the ratio of each surface conditioning agent；
（8）Separating twice, classification are processed and packed, and obtain highly active nano-calcium carbonate.
2. the preparation method of the high-activity nano calcium carbonate of a kind of surface-active-treatment according to claim 1, its feature
It is, the step（1）Solution temperature is 50 DEG C~60 DEG C after the dilution of middle nano-calcium carbonate emulsion, solution concentration is 8.0%~
10.0%。
3. the preparation method of the high-activity nano calcium carbonate of a kind of surface-active-treatment according to claim 1, its feature
It is, the step（2）Prepared by middle neat soap solution, the neat soap solution temperature after hot water dissolving is 80 DEG C~100 DEG C, after dissolving
The solution concentration of neat soap solution is 10.0%~15.0%, and lipid activating agent is 10%~50% coconut oil.
4. the preparation method of the high-activity nano calcium carbonate of a kind of surface-active-treatment according to claim 1, its feature
It is, the step（3）Prepared by middle soap emulsion, temperature is 80 DEG C~100 DEG C after fatty acid mixed proportioning hot water dissolving,
The solution concentration of soap emulsion is 20.0%~25.0%, and concentration of sodium hydroxide solution is 30%~35%.
5. the preparation method of the high-activity nano calcium carbonate of a kind of surface-active-treatment according to claim 1, its feature
It is, the step（4）Middle wet process surface treatment process temperature is controlled between 40-80 DEG C, and surface conditioning agent quality is carbonic acid
The 2.0%~5.0% of calcareous amount.
6. the preparation method of the high-activity nano calcium carbonate of a kind of surface-active-treatment according to claim 1, its feature
It is, the step（7）Between 80-110 DEG C, surface conditioning agent quality is carbon to the temperature control of middle dry surface processing procedure
The 0.4%~2.0% of the calcareous amount of acid.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN115849425A (en) * | 2022-12-09 | 2023-03-28 | 安徽省宣城市华纳新材料科技有限公司 | Preparation method of nano calcium carbonate for low-modulus high-elasticity silicone adhesive |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN115849425A (en) * | 2022-12-09 | 2023-03-28 | 安徽省宣城市华纳新材料科技有限公司 | Preparation method of nano calcium carbonate for low-modulus high-elasticity silicone adhesive |
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Application publication date: 20170517 |