CN108912741A - A kind of preparation process of ultra-fine surface modified nano calcium carbonate - Google Patents
A kind of preparation process of ultra-fine surface modified nano calcium carbonate Download PDFInfo
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- CN108912741A CN108912741A CN201810791023.7A CN201810791023A CN108912741A CN 108912741 A CN108912741 A CN 108912741A CN 201810791023 A CN201810791023 A CN 201810791023A CN 108912741 A CN108912741 A CN 108912741A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
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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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/90—Other properties not specified above
Abstract
The invention discloses a kind of preparation processes of ultra-fine surface modified nano calcium carbonate, include the following steps：(1) calcium hydroxide suspension is carbonized, and sodium sulphate and sodium citrate mixing morphology regulation additives is added, until slurry pH=7.0, obtains nanometer calcium carbonate slurry；(2) dispersing agent is added into nanometer calcium carbonate slurry, stirs simultaneously temperature control, heat preservation；(3) surface modifier, temperature control and sonic oscillation are added into step (2) nanometer calcium carbonate slurry；(4) the nanometer calcium carbonate slurry after surface treatment is obtained into the ultra-fine surface modified nano calcium carbonate of finished product successively through filters pressing and centrifugal dehydration, drying, depolymerization and sieving.Preparation process of the invention can prevent nanometer calcium carbonate from reuniting, the hydrophobicity and compatibility on nanometer calcium carbonate surface are enhanced, makes it easier to disperse in the polymer, stearic acid soda soap liquid had not only been used as emulsifier but also had been used as saponification agent in preparation process, it is high to react saponification rate, raw material availability is high.
Description
Technical field
The present invention relates to calcium carbonate preparation technical field, in particular to a kind of preparation of ultra-fine surface modified nano calcium carbonate
Technique.
Background technique
Calcium carbonate is a kind of widely used inorganic chemicals industry product, can be used as filling and modified modifying material, industrially
It is usually used in having for the industries such as plastics, rubber, paint, adhesive, papermaking and food processing, pharmacy with daily life
Close relationship.
Nanometer calcium carbonate refers to that size in the calcium carbonate of nanometer scale, can be divided into spindle, needle-like, ball from crystal form
Type, Cubic, chain etc. are a kind of Novel super-thin solid inorganic chemical materials to grow up the 1980s.Due to receiving
The fine of rice calcium carbonate particle, crystal structure and Electronic Structure are changed, and produce ordinary calcium carbonate institute not
Small-size effect, surface and interfacial effect, quantum size effect, the macro quanta tunnel effect having, magnetism, catalyst,
Photo-thermal resistance and fusing point etc. have performance more superior than conventional material.
When nanometer calcium carbonate directly applies to industrial products, due to its surface hydrophilic oleophobic, in highly polar, in organic media
In be difficult to it is evenly dispersed, it is poor with the binding force of base-material, easily cause boundary defect, material property caused to decline；In addition, nano-calcium carbonate
Calcium particle partial size is smaller, and the atomicity on surface is more, and surface can be higher, and suction-operated is stronger, is in the unstable shape of thermodynamics
State is easily reunited mutually between each particle, can not be dispersed well in a polymer matrix, to influence the practical application of nanoparticle
Effect.
Currently, industrial method of modifying includes dry method modification and wet-process modified, wherein wet-process modified mainly use fatty acid
(salt) is surface modifier, but fatty acid (salt) has stronger hydrophobic effect, needs higher mechanical force and higher temperature ability
Obtain preferable dispersion effect, but to will cause cost excessively high for such surface treatment process, and nanometer calcium carbonate is locally reunited
It is difficult to solve, hard aggregation is inevitable between particle.
Summary of the invention
The present invention is in view of the deficienciess of the prior art, provide a kind of preparation work of ultra-fine surface modified nano calcium carbonate
Skill, specific technical solution are as follows：
A kind of preparation process of ultra-fine surface modified nano calcium carbonate, includes the following steps：
(1) it is passed through carbon dioxide into calcium hydroxide suspension to be carbonized, and sodium sulphate and sodium citrate is added simultaneously
Morphology regulation additives are mixed, until slurry pH=7.0, obtains nanometer calcium carbonate slurry；
(2) dispersing agent is added into nanometer calcium carbonate slurry, stirs simultaneously temperature control, keeps the temperature 20~30min；
(3) surface modifier, temperature control and 30~60min of sonic oscillation are added into step (2) nanometer calcium carbonate slurry；
(4) by the nanometer calcium carbonate slurry after surface treatment successively through filters pressing and centrifugal dehydration, drying, depolymerization and mistake
Sieve, obtains the ultra-fine surface modified nano calcium carbonate of finished product.
As a further improvement of the present invention, dispersing agent is vinyl bis-stearamides, N- stearyl in the step (2)
At least one of erucyl amide, sulfobetaines.
As a further improvement of the present invention, stirring rate is 100~200r/min in the step (2).
As a further improvement of the present invention, whipping temp is 40~60 DEG C in the step (2).
As a further improvement of the present invention, the preparation method of the surface modifier in the step (3) is：By deionization
Water is heated to 100 DEG C, adds stearic acid soda soap liquid, is stirring evenly and then adding into stearic acid, reacts 3~5h, is eventually adding addition caustic soda,
Washing, dehydration, surface modifier obtained by drying.
As a further improvement of the present invention, the concentration of stearic acid soda soap liquid is in the preparation method of the surface modifier
25~45%.
As a further improvement of the present invention, the frequency of sonic oscillation is 200~300kHz in the step (3).
As a further improvement of the present invention, temperature control is 50~60 DEG C in the step (3).
Beneficial effects of the present invention：The present invention is carrying out nanometer calcium carbonate tentatively to live to it before surface is modified
Change, the nanometer calcium carbonate with mobility and dispersibility is obtained using the polymolecularity and compatibility of dispersing agent, prevents nano-sized carbon
Sour calcium is reunited, and the mechanical resistance in Process of Surface Modification is reduced, and improves the performance of later period modified nano calcium carbonate；It is modified to receive
Rice calcium carbonate surface has coated stearate, and forms chemisorption with nanometer calcium carbonate, enhances nanometer calcium carbonate surface
Hydrophobicity makes it easier to disperse in the polymer, reduces the reunion of nanoparticle；It is prepared by modified stearate used
Cheng Zhong, stearic acid soda soap liquid be not only used as emulsifier but also be used as saponification agent, and reaction saponification rate is high, and raw material availability is high.
Detailed description of the invention
Fig. 1 is the corresponding oil absorbency of various embodiments of the present invention, viscosity and contact angle；
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
A kind of preparation process of ultra-fine surface modified nano calcium carbonate, includes the following steps：
(1) 3m is passed through into 300kg calcium hydroxide suspension3/ min carbon dioxide is carbonized, and 2kg sulphur is added simultaneously
Sour sodium obtains nanometer calcium carbonate slurry up to slurry pH=7.0 with sodium citrate mixing morphology regulation additives；
(2) 2.5kg vinyl bis-stearamides are added into nanometer calcium carbonate slurry, simultaneously temperature control 40 is mixed with 100r/min
DEG C, keep the temperature 20~30min；
(3) ultrasound under the addition 4kg surface modifier into step (2) nanometer calcium carbonate slurry, 50 DEG C of temperature control and 200kHz
Vibrate 30min；
(4) by the nanometer calcium carbonate slurry after surface treatment successively through filters pressing and centrifugal dehydration, drying, depolymerization and mistake
Sieve, obtains the ultra-fine surface modified nano calcium carbonate of finished product.
In the present embodiment, the preparation method of the surface modifier is：Deionized water is heated to 100 DEG C, adds the concentration to be
25% stearic acid soda soap liquid is stirring evenly and then adding into stearic acid, reacts 3h, is eventually adding addition caustic soda, and washing, is dried at dehydration
Dry surface modifier to obtain the final product.
Embodiment 2
A kind of preparation process of ultra-fine surface modified nano calcium carbonate, includes the following steps：
(1) 3m is passed through into 300kg calcium hydroxide suspension3The carbon dioxide of/min is carbonized, and 2kg is added simultaneously
Sodium sulphate obtains nanometer calcium carbonate slurry up to slurry pH=7.0 with sodium citrate mixing morphology regulation additives；
(2) 2.5kgN- stearyl erucamide is added into nanometer calcium carbonate slurry, simultaneously temperature control 50 is mixed with 150r/min
DEG C, keep the temperature 25min；
(3) ultrasound under the addition 4kg surface modifier into step (2) nanometer calcium carbonate slurry, 55 DEG C of temperature control and 250kHz
Vibrate 45min；
(4) by the nanometer calcium carbonate slurry after surface treatment successively through filters pressing and centrifugal dehydration, drying, depolymerization and mistake
Sieve, obtains the ultra-fine surface modified nano calcium carbonate of finished product.
In the present embodiment, the preparation method of the surface modifier is：Deionized water is heated to 100 DEG C, adds the concentration to be
35% stearic acid soda soap liquid is stirring evenly and then adding into stearic acid, reacts 4h, is eventually adding addition caustic soda, and washing, is dried at dehydration
Dry surface modifier to obtain the final product.
Embodiment 3
A kind of preparation process of ultra-fine surface modified nano calcium carbonate, includes the following steps：
(1) 3m is passed through into 300kg calcium hydroxide suspension3The carbon dioxide of/min is carbonized, and 2kg is added simultaneously
Sodium sulphate obtains nanometer calcium carbonate slurry up to slurry pH=7.0 with sodium citrate mixing morphology regulation additives；
(2) 2.5kg sulfobetaines is added into nanometer calcium carbonate slurry, mixes simultaneously 60 DEG C of temperature control with 200r/min, heat preservation
30min；
(3) 4kg surface modifier is added into step (2) nanometer calcium carbonate slurry, 60 DEG C of temperature control simultaneously surpasses under 300kHz
Sound oscillation 60min；
(4) by the nanometer calcium carbonate slurry after surface treatment successively through filters pressing and centrifugal dehydration, drying, depolymerization and mistake
Sieve, obtains the ultra-fine surface modified nano calcium carbonate of finished product.
In the present embodiment, the preparation method of the surface modifier is：Deionized water is heated to 100 DEG C, adds the concentration to be
45% stearic acid soda soap liquid is stirring evenly and then adding into stearic acid, reacts 5h, is eventually adding addition caustic soda, and washing, is dried at dehydration
Dry surface modifier to obtain the final product.
Comparative example 1
A kind of preparation process of ultra-fine surface modified nano calcium carbonate, includes the following steps：
(1) 3m is passed through into 300kg calcium hydroxide suspension3/ min carbon dioxide is carbonized, and 2kg sulphur is added simultaneously
Sour sodium obtains nanometer calcium carbonate slurry up to slurry pH=7.0 with sodium citrate mixing morphology regulation additives；
(2) 4kg surface modifier, 60 DEG C of temperature control and the sonic oscillation under 300kHz are added into nanometer calcium carbonate slurry
60min；
(3) by the nanometer calcium carbonate slurry after surface treatment successively through filters pressing and centrifugal dehydration, drying, depolymerization and mistake
Sieve, obtains the ultra-fine surface modified nano calcium carbonate of finished product.
In the present embodiment, the preparation method of the surface modifier is：Deionized water is heated to 100 DEG C, adds the concentration to be
45% stearic acid soda soap liquid is stirring evenly and then adding into stearic acid, reacts 5h, is eventually adding addition caustic soda, and washing, is dried at dehydration
Dry surface modifier to obtain the final product.
Comparative example 2
A kind of preparation process of ultra-fine surface modified nano calcium carbonate, includes the following steps：
(1) 3m is passed through into 300kg calcium hydroxide suspension3/ min carbon dioxide is carbonized, and 2kg sulphur is added simultaneously
Sour sodium obtains nanometer calcium carbonate slurry up to slurry pH=7.0 with sodium citrate mixing morphology regulation additives；
(2) nanometer calcium carbonate slurry is obtained into the ultra-fine table of finished product successively through filters pressing and centrifugal dehydration, drying, depolymerization and sieving
Face modified nano calcium carbonate.
Ultra-fine surface modified nano calcium carbonate resulting to Examples 1 to 3 and comparative example 1,2 carries out DATA REASONING, in detail
See Fig. 1.Fig. 1 shows that dispersing agent can improve oil absorbency, viscosity and the contact angle of nanometer calcium carbonate to a certain extent, and surface
Modifying agent is in the properties for fundamentally changing nanometer calcium carbonate, so that nanometer calcium carbonate is that can generate more preferably as filler
Reinforcing effect.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (8)
1. a kind of preparation process of ultra-fine surface modified nano calcium carbonate, which is characterized in that include the following steps：
(1) it is passed through carbon dioxide into calcium hydroxide suspension to be carbonized, and sodium sulphate is added simultaneously and is mixed with sodium citrate
Morphology regulation additives, until slurry pH=7.0, obtains nanometer calcium carbonate slurry；
(2) dispersing agent is added into nanometer calcium carbonate slurry, stirs simultaneously temperature control, keeps the temperature 20~30min；
(3) surface modifier, temperature control and 30~60min of sonic oscillation are added into step (2) nanometer calcium carbonate slurry；
(4) by the nanometer calcium carbonate slurry after surface treatment successively through filters pressing and centrifugal dehydration, drying, depolymerization and sieving,
Obtain the ultra-fine surface modified nano calcium carbonate of finished product.
2. a kind of preparation process of ultra-fine surface modified nano calcium carbonate as described in claim 1, which is characterized in that the step
Suddenly dispersing agent is at least one of vinyl bis-stearamides, N- stearyl erucamide, sulfobetaines in (2).
3. a kind of preparation process of ultra-fine surface modified nano calcium carbonate as described in claim 1, which is characterized in that the step
Suddenly stirring rate is 100~200r/min in (2).
4. a kind of preparation process of ultra-fine surface modified nano calcium carbonate as described in claim 1, which is characterized in that the step
Suddenly whipping temp is 40~60 DEG C in (2).
5. a kind of preparation process of ultra-fine surface modified nano calcium carbonate as described in claim 1, which is characterized in that the step
Suddenly the preparation method of the surface modifier in (3) is：Deionized water is heated to 100 DEG C, adds stearic acid soda soap liquid, stirs evenly
After be added stearic acid, react 3~5h, be eventually adding addition caustic soda, washing, dehydration, surface modifier obtained by drying.
6. a kind of preparation process of ultra-fine surface modified nano calcium carbonate as described in claim 1, which is characterized in that the table
The concentration of stearic acid soda soap liquid is 25~45% in the preparation method of face modifying agent.
7. a kind of preparation process of ultra-fine surface modified nano calcium carbonate as described in claim 1, which is characterized in that the step
Suddenly the frequency of sonic oscillation is 200~300kHz in (3).
8. a kind of preparation process of ultra-fine surface modified nano calcium carbonate as described in claim 1, which is characterized in that the step
Suddenly temperature control is 50~60 DEG C in (3).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109399682A (en) * | 2018-12-06 | 2019-03-01 | 河南省科学院高新技术研究中心 | A kind of food additives active nano-calcium carbonate and preparation method thereof |
| CN109516485A (en) * | 2018-12-06 | 2019-03-26 | 河南省科学院高新技术研究中心 | A kind of method that self-emulsifying systems prepare rodlike modified calcium carbonate |
| CN111909424A (en) * | 2020-07-07 | 2020-11-10 | 广西夏阳环保科技有限公司 | Preparation method and application of modified nano calcium carbonate for rubber |
| CN112960685A (en) * | 2021-03-04 | 2021-06-15 | 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 hard PVC (polyvinyl chloride) |
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| CN106317963A (en) * | 2016-08-22 | 2017-01-11 | 江西广源化工有限责任公司 | Preparation method of modified calcium carbonate |
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| CN1161703A (en) * | 1994-08-29 | 1997-10-08 | 卡伯特公司 | Universal masterbatch |
| CN101774623A (en) * | 2010-01-19 | 2010-07-14 | 上海卓越纳米新材料股份有限公司 | Industrial preparation method of rice-shaped ultra-fine activated calcium carbonate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109399682A (en) * | 2018-12-06 | 2019-03-01 | 河南省科学院高新技术研究中心 | A kind of food additives active nano-calcium carbonate and preparation method thereof |
| CN109516485A (en) * | 2018-12-06 | 2019-03-26 | 河南省科学院高新技术研究中心 | A kind of method that self-emulsifying systems prepare rodlike modified calcium carbonate |
| CN111909424A (en) * | 2020-07-07 | 2020-11-10 | 广西夏阳环保科技有限公司 | Preparation method and application of modified nano calcium carbonate for rubber |
| CN111909424B (en) * | 2020-07-07 | 2022-06-17 | 都安春旭新材料科技有限责任公司 | Preparation method and application of modified nano calcium carbonate for rubber |
| CN112960685A (en) * | 2021-03-04 | 2021-06-15 | 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 hard PVC (polyvinyl chloride) |
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