CN106433220A - Preparation method of modified superfine calcium carbonate powder and product of preparation method - Google Patents
Preparation method of modified superfine calcium carbonate powder and product of preparation method Download PDFInfo
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- CN106433220A CN106433220A CN201610694859.6A CN201610694859A CN106433220A CN 106433220 A CN106433220 A CN 106433220A CN 201610694859 A CN201610694859 A CN 201610694859A CN 106433220 A CN106433220 A CN 106433220A
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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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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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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Abstract
The invention provides a preparation method of modified superfine calcium carbonate powder. The preparation method comprises following steps: raw material mixing, slurry preparation, wet grinding, drying collection, depolymerization scattering and modified treatment, wherein a dispersing agent at least comprises ammonium polyacrylate salt, sodium hexametaphosphate and sodium polyacrylate salt; a modifying agent comprises one or more of octadecylamine, polymethyl methacrylate, a titanate coupling agent and a silane coupling agent; and a hyperdispersant comprises one or more of a polyester type hyperdispersant, a polyether type hyperdispersant, a polyacrylate hyperdispersant and a polyolefin hyperdispersant. By virtue of the preparation method, the dispersity of the powder can be improved, the dry-wet cover effects of building coatings can be improved, and the addition amount of titanium dioxide can be reduced.
Description
【Technical field】
The present invention relates to modified calcium carbonate powder technology field, the more particularly, to ultra-fine carbonic acid of the special modification of building coating
Calcium raw powder's production technology and its product.
【Background technology】
Calcium Carbonate (Calcium Carbonate) is a kind of important, broad-spectrum inorganic salt.Ground calcium carbonate
(Heavy Calcium Carbonate) is also known as grinding calcium carbonate (Ground Calcium Carbonate, abbreviation GCC, the U.S.
Claim Kotamite), it is mechanically directly to pulverize natural calcite, marble, limestone etc. and be obtained.Due to sinking of it
Fall volume (1.1-1.9mL/g/g) is less, therefore than the precipitated calcium carbonate settling volume (2.4-2.8mL/g) chemically producing
It is referred to as ground calcium carbonate.
Ground calcium carbonate can be divided into corase grind Calcium Carbonate (more than 3 μm), fine grinding Calcium Carbonate (1～3 μ by its original mean diameter
M), calcium carbonate superfine powder (0.5～1 μm).Superfine heavy calcium carbonate has that chemical purity is high, inertia is big, is difficult chemical reaction, heat is steady
Qualitative good, will not decompose below 400 DEG C, whiteness is high, oil absorbency is low, index of refraction is low, matter is soft, drys, do not contain water of crystallization, no
Malicious, tasteless, odorless, cheap the advantages of, be widely used in paint, ink, coating, plastics, rubber, papermaking, cable, pottery
The fields such as porcelain, glass, electronics, cosmetics, medicine, food, playing as filler increases referring to, reducing production cost of product
Effect.
However, the common extra fine heavy calcium carbonate powder body surface activity of itself is big, easily reunite, bad dispersibility, therefore
It is impossible to give full play to its space steric effect when being added in building coating (as emulsion paint) as filler, thus cannot have
Effect improves the dry and wet covering effect of building coating, reduces the addition of titanium dioxide in formula, has had a strong impact on its own excellent
Performance and application effect of products.
【Content of the invention】
For drawbacks described above of the prior art, the invention provides a kind of preparation side of modified calcium carbonate superfine powder powder body
Method, it is possible to increase the dispersibility of powder body, improves the dry and wet covering effect of building coating, reduces the addition of titanium dioxide.
The technical scheme is that：
A kind of modified calcium carbonate superfine powder raw powder's production technology is it is characterised in that comprise the following steps：
1) raw material mixing：By calcite and Kaolin mixed grinding, obtain the composite granule of 400～600 mesh；
2) prepare slurry：By step 1) composite granule that obtains become with the solution of dispersant solid content be 75～
85% slurry, described dispersant comprises one or more of ammonium polyacrylate salt, sodium hexameta phosphate and polyacrylic acid sodium salt；
3) wet grinding：By step 2) slurry that obtains carries out wet grinding, obtains the slurry of 8000-10000 mesh；
4) it is dried and collect：Through step 3) slurry drying that obtains is less than 0.2% to moisture, and collect and powder body is dried；
5) depolymerization is broken up：By step 4) obtain be dried powder body enter Depolymerizing thrasher, with the speed of 1500-2500r/min
Degree is broken up, and obtains depolymerization powder body；
6) modification：By step 5) the depolymerization powder body that obtains enters surface modification machine, adds modifying agent and hyper-dispersant
Carry out cladding process, temperature is 75-85 DEG C, by the friction between powder body and modifying agent, produce cladding, modification time is 20-
40min, obtains final product；Described modifying agent comprises octadecylamine, polymethyl methacrylate, titanate coupling agent and silicon
One or more of alkane coupling agent；Described hyper-dispersant comprises polyester type ultra-dispersant agent, polyether-type hyper-dispersant, polyacrylic acid
One or more of ester hyper-dispersant and polyolefin hyper-dispersant.
Specifically, above-mentioned steps 1) in calcite and kaolinic mass ratio be (50～100)：1.Using kaolinic
Laminated structure, can make Calcium Carbonate more fully be disperseed, simultaneously because the refractive index of Kaolin itself is higher, therefore compound
The refractive index of composite granule can be lifted afterwards, but because Kaolin oil absorption itself is higher, so accounting is unsuitable too high, comprehensively examine
Consider factors above, calcite and kaolinic mass ratio are preferably (50～100)：1.
Specifically, above-mentioned steps 2) in the mass ratio of ammonium polyacrylate salt, sodium hexameta phosphate and polyacrylic acid sodium salt be
(6～9)：1：(4～7).In this proportion, several dispersants can reach preferably cold spelling effect.
Specifically, above-mentioned steps 2) in the addition of dispersant be 6～the 9 ‰ of calcite and Kaolin gross mass.Point
Powder adds excessively, and during more than 10 ‰, during by applying filler in building coating, the resistance to water of paint film can be affected, and adds
When measuring very few, during less than 5 ‰, grinding-aid effect is inconspicuous, and powder body dispersion effect is not good.
Specifically, above-mentioned steps 3) to grind for constant temperature, temperature is 40-60 DEG C, and grinding rate is 250-350r/min, at this
Under parameter, grinding efficiency is up to maximization.
Specifically, above-mentioned steps 6) modifying agent in octadecylamine, polymethyl methacrylate, titanate coupling agent and
The addition of silane coupler is respectively 1 ‰～3 ‰, 1 ‰～2 ‰, 3 ‰～9 ‰ and 1 ‰～the 3 ‰ of powder quality, just may be used
With complete covered composite yarn powder body, excessive or how much all can affect covered effect.
Specifically, above-mentioned steps 6) hyper-dispersant addition be powder quality 2 ‰～5 ‰.Within the range, surpass
Dispersant just can act on composite granule completely, reaches optimal cost performance.
Specifically, above-mentioned steps 6) hyper-dispersant in polyester type ultra-dispersant agent, polyether-type hyper-dispersant, polyacrylic acid
The mass ratio of ester hyper-dispersant and polyolefin hyper-dispersant is 1：(2～5)：(1～3)：(1～4).Within this range, Ji Zhongchao
The cold spelling effect of dispersant preferably, can give full play to the effect of various hyper-dispersants.
A kind of product that above-mentioned modified calcium carbonate superfine powder raw powder's production technology obtains is it is characterised in that described product
Refractive index be 1.60-1.62, covering effect preferably, can reduce the consumption of titanium dioxide further.
Further, the mean diameter of above-mentioned product is 0.5-1 μm, by the superfine powder of dry grinding and wet grinding
Powder granule can be ground to 10000 mesh by processing technique, has less particle diameter with respect to conventional grinding.
The present invention has following beneficial technique effect：
(1) good dispersion：The present invention adopts composite modified technique, adds dispersant, beat in depolymerization in preparing slurry
Add modifying agent and hyper-dispersant, three's compounding use after dissipating, can effectively play the not same-action of various auxiliary agents, take long benefit
Short, cold spelling auxiliary agent, thus reach preferably modified dispersion effect, such as this product and water in mass ratio 1:After 1 is made into slurry, standing
In in the air, can keep one month becoming suspension emulsion, not precipitate, non-modified calcium carbonate product will within one day
Precipitate.
(2) fully, result of prevention is good for Surface coating；The present invention adopts composite modified technique, carries out after depolymerization is broken up
Surface treatment, adopts multiple water such as silane coupler, titanate coupling agent, octadecylamine, polymethyl methacrylate simultaneously
Property modifying agent carry out surface coating modification, modified effect is splendid, and the surface coating rate of product is more than 99%, compatible with water-based system
Property good, be simultaneously introduced several hyper-dispersants to improve the dispersibility of powder body, composite granule water can be kept into suspension breast
Liquid one month, when being applied in building coating, can effectively improve the storage stability of product, product in water-based system with
Water is sufficiently mixed, and forms suspension emulsion, should not settle, result of prevention is excellent.
(3) fineness is thin：The present invention passes through the super fine powder processing technique of dry grinding and wet grinding, can be by powder body
Grain is ground to 10000 mesh, and at 0.5-1 μm, BET specific surface area is more than 17m to its mean diameter2/g.Simultaneously in product processes
Employ the technique that depolymerization is broken up, effectively solve the agglomeration traits of granule, maintain the particle diameter of primary partical.Diameter of particle
Thinner, it is used cooperatively with titanium dioxide and more can play its extending effect, particularly when diameter of particle and titanium dioxide particle diameter are close,
The distribution of space steric effect extension titanium dioxide can farthest be passed through, play the covering effect of titanium dioxide to the full extent
Should.
(4) refractive index is high, and extending effect is good：The present invention adopts calcite and the Kaolin collocation of certain mass ratio to use,
Add various dispersants and hyper-dispersant, the refraction of the product of preparation in wet grinding process and later stage modifying process simultaneously
Rate brings up to 1.60-1.62.(refractive index of ordinary calcium carbonate is 1.58, and barite is 1.62.) this products application in building apply
When in material, dry powder covering effect is good, simultaneously because the collocation of various dispersant and hyper-dispersant uses, can preferably play it and prolong
Exhibition effect, gives full play to the covering power of titanium dioxide, reduces production cost.
【Brief description】
Fig. 1 is the flow chart of the preparation method of the present invention.
【Specific embodiment】
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment provided below simultaneously is not used to limit the scope that the present invention is covered, and described step is not to use
To limit its execution sequence.Those skilled in the art do conspicuously improved with reference to existing common knowledge to the present invention, also fall
Enter within the protection domain of application claims.
Embodiment one
Calcite ore and Kaolin are with 100:1 ratio is crushed, and wears into the dry powder of 400 mesh, is configured to admittedly contain
Measure the slurry for 80%, add ammonium polyacrylate salt, sodium hexameta phosphate and three kinds of dispersants of polyacrylic acid sodium salt, dispersant accounts for dry
The 6% of powder mass fraction, the ratio of three kinds of dispersants is 6:1:7.Slurry injection 3600L vertical wet-process grinder after scattered
In carry out wet grinding, wear into the slurry in 10000 mesh for the fineness, after expansion drying through cloth bag collect, add beater in carry out
Depolymerization is broken up so as to keep the primary particle diameter of granule, is then added in surface modification machine by spiral reamer, is separately added into
The solid state modification agent of certain powder quality ratio, liquid modifier and hyper-dispersant, carry out parcel process, improve its dispersion further
Effect, it is to avoid the secondary agglomeration of primary particle diameter.Wherein, solid state modification agent is 1 ‰ octadecylamines, 1 ‰ poly-methyl methacrylates
Ester, liquid modifier is 3 ‰ titanate coupling agents, 1 ‰ silane couplers；Hyper-dispersant is respectively polyester type ultra-dispersant agent, gathers
Ether type hyper-dispersant, polyacrylate hyper-dispersant and polyolefin hyper-dispersant, its addition accounts for the 2 ‰ of powder quality, adds
Plus ratio is polyester type ultra-dispersant agent：Polyether-type hyper-dispersant：Polyacrylate hyper-dispersant：Polyolefin hyper-dispersant=1:
2:1:4.
Composite modified rear product is packaged into final finished through automatic packaging machine after sieving.Shown by scanning electron microscopic observation,
The surface coating rate of this product is more than 98%.This product and water in mass ratio 1:After 1 is made into slurry, it is statically placed in the air, can protect
Hold one month and become suspension emulsion, do not precipitate, and non-modified calcium carbonate product will precipitate within one day.
Embodiment two
Calcite ore and Kaolin are with 80:1 ratio is crushed, and wears into the dry powder of 400 mesh, is configured to solid content
Slurry for 80%, adds ammonium polyacrylate salt, sodium hexameta phosphate and three kinds of dispersants of polyacrylic acid sodium salt, and dispersant accounts for dry powder
The 6% of mass fraction, the ratio of three kinds of dispersants is 9:1:4.In slurry injection 3600L vertical wet-process grinder after scattered
Carry out wet grinding, wear into the slurry in 8000 mesh for the fineness, collect through cloth bag after expansion drying, add in beater and carry out depolymerization
Break up so as to keep the primary particle diameter of granule, then added in surface modification machine by spiral reamer, be separately added into certain
The solid state modification agent of powder quality ratio, liquid modifier and hyper-dispersant, carry out parcel process, improve its dispersion effect further
Really, it is to avoid the secondary agglomeration of primary particle diameter.Wherein, solid state modification agent is 2 ‰ octadecylamines, 1 ‰ polymethyl methacrylates,
Liquid modifier is 2 ‰ titanate coupling agents, 2 ‰ silane couplers；Hyper-dispersant is respectively polyester type ultra-dispersant agent, polyether-type
Hyper-dispersant, polyacrylate hyper-dispersant and polyolefin hyper-dispersant, its addition accounts for the 3 ‰ of powder quality, adds ratio
Example is polyester type ultra-dispersant agent：Polyether-type hyper-dispersant：Polyacrylate hyper-dispersant：Polyolefin hyper-dispersant=1:3:1:
2.
Composite modified rear product is packaged into final finished through automatic packaging machine after sieving.This product and water in mass ratio 1:1
After being made into slurry, it is statically placed in the air, can keep one month becoming suspension emulsion, not precipitate, and non-modified carbonic acid
Calcium product will precipitate within one day.
Embodiment three
Calcite ore and Kaolin are with 50:1 ratio is crushed, and wears into the dry powder of 400 mesh, is configured to solid content
Slurry for 80%, adds ammonium polyacrylate salt, sodium hexameta phosphate and three kinds of dispersants of polyacrylic acid sodium salt, and dispersant accounts for dry powder
The 6% of mass fraction, the ratio of three kinds of dispersants is 4:1:5.In slurry injection 3600L vertical wet-process grinder after scattered
Carry out wet grinding, wear into the slurry in 9000 mesh for the fineness, collect through cloth bag after expansion drying, add in beater and carry out depolymerization
Break up so as to keep the primary particle diameter of granule, then added in surface modification machine by spiral reamer, be separately added into certain
The solid state modification agent of powder quality ratio, liquid modifier and hyper-dispersant, carry out parcel process, improve its dispersion effect further
Really, it is to avoid the secondary agglomeration of primary particle diameter.Wherein, solid state modification agent is 1 ‰ octadecylamines, 2 ‰ polymethyl methacrylates,
Liquid modifier is 1 ‰ titanate coupling agents, 3 ‰ silane couplers；Hyper-dispersant is respectively polyester type ultra-dispersant agent, polyether-type
Hyper-dispersant, polyacrylate hyper-dispersant and polyolefin hyper-dispersant, its addition accounts for the 2 ‰ of powder quality fraction, adds
Plus ratio is polyester type ultra-dispersant agent：Polyether-type hyper-dispersant：Polyacrylate hyper-dispersant：Polyolefin hyper-dispersant=1:
4:2:3.
Composite modified rear product is packaged into final finished through automatic packaging machine after sieving.This product and water in mass ratio 1:1
After being made into slurry, it is statically placed in the air, can keep one month becoming suspension emulsion, not precipitate, and non-modified carbonic acid
Calcium product will precipitate within one day.
The performance of the calcium carbonate superfine powder powder body of the modification obtaining in above example is as follows：
Claims (10)
1. a kind of modified calcium carbonate superfine powder raw powder's production technology is it is characterised in that comprise the following steps：
1) raw material mixing：By calcite and Kaolin mixed grinding, obtain the composite granule of 400～600 mesh；
2) prepare slurry：By step 1) composite granule that obtains becomes solid content to be 75～85% with the solution of dispersant
Slurry, described dispersant comprises one or more of ammonium polyacrylate salt, sodium hexameta phosphate and polyacrylic acid sodium salt；
3) wet grinding：By step 2) slurry that obtains carries out wet grinding, obtains the slurry of 8000-10000 mesh；
4) it is dried and collect：Through step 3) slurry drying that obtains is less than 0.2% to moisture, and collect and powder body is dried；
5) depolymerization is broken up：By step 4) obtain be dried powder body enter Depolymerizing thrasher, beaten with the speed of 1500-2500r/min
Dissipate, obtain depolymerization powder body；
6) modification：By step 5) the depolymerization powder body that obtains enters surface modification machine, adds modifying agent and hyper-dispersant to carry out
Cladding is processed, and temperature is 75-85 DEG C, and modification time is 20-40min, obtains final product；Described modifying agent comprises octadecyl
One or more of amine, polymethyl methacrylate, titanate coupling agent and silane coupler；Described hyper-dispersant comprises to gather
One or more of ester type hyper-dispersant, polyether-type hyper-dispersant, polyacrylate hyper-dispersant and polyolefin hyper-dispersant.
2. modified calcium carbonate superfine powder raw powder's production technology according to claim 1 is it is characterised in that described step 1)
In calcite and kaolinic mass ratio be (50～100)：1.
3. modified calcium carbonate superfine powder raw powder's production technology according to claim 1 is it is characterised in that described step 2)
In ammonium polyacrylate salt, sodium hexameta phosphate and polyacrylic acid sodium salt mass ratio be (6～9)：1：(4～7).
4. the calcium carbonate superfine powder raw powder's production technology of the modification according to claim 1 or 3 is it is characterised in that described step
The addition of the dispersant in rapid 2) is 6～the 9 ‰ of calcite and Kaolin gross mass.
5. modified calcium carbonate superfine powder raw powder's production technology according to claim 1 is it is characterised in that described step 3)
Grind for constant temperature, temperature is 40-60 DEG C, grinding rate is 250-350r/min.
6. modified calcium carbonate superfine powder raw powder's production technology according to claim 1 is it is characterised in that described step 6)
Modifying agent in octadecylamine, the addition of polymethyl methacrylate, titanate coupling agent and silane coupler be respectively
The 1 ‰ of powder quality～3 ‰, 1 ‰～2 ‰, 3 ‰～9 ‰ and 1 ‰～3 ‰.
7. modified calcium carbonate superfine powder raw powder's production technology according to claim 1 is it is characterised in that described step 6)
Hyper-dispersant addition be powder quality 2 ‰～5 ‰.
8. modified calcium carbonate superfine powder raw powder's production technology according to claim 1 is it is characterised in that described step 6)
Hyper-dispersant in polyester type ultra-dispersant agent, polyether-type hyper-dispersant, polyacrylate hyper-dispersant and polyolefin ultra-dispersed
The mass ratio of agent is 1：(2～5)：(1～3)：(1～4).
9. the product that a kind of calcium carbonate superfine powder raw powder's production technology of the modification as described in any one as claim 1-8 obtains,
It is characterized in that, the refractive index of described product is 1.60-1.62.
10. product according to claim 9 is it is characterised in that the mean diameter of described product is 0.5-1 μm.
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Cited By (18)
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| CN106071690A (en) * | 2016-06-20 | 2016-11-09 | 柳州市美食联盟协会 | A kind of coarse grain porridge |
| CN107488280A (en) * | 2017-09-30 | 2017-12-19 | 广西华洋矿源材料有限公司 | A kind of preparation method of calcium carbonate superfine powder and rubber composite |
| CN107541095A (en) * | 2017-07-21 | 2018-01-05 | 贺州钟山县双文碳酸钙新材料有限公司 | A kind of ultrawhite calcium carbonate |
| CN108752979A (en) * | 2018-05-10 | 2018-11-06 | 桂林永福恒达实业有限公司 | A kind of method that wet method prepares super fine calcium carbonate |
| CN108929570A (en) * | 2018-05-10 | 2018-12-04 | 桂林永福恒达实业有限公司 | A kind of method of wet production super fine calcium carbonate |
| CN109294279A (en) * | 2018-09-13 | 2019-02-01 | 浙江钦堂钙业股份有限公司 | A kind of high-performance powder and its production method |
| CN110697752A (en) * | 2019-09-22 | 2020-01-17 | 佛山市展华科技有限公司 | Modification method of nano calcium carbonate |
| CN110791260A (en) * | 2019-11-15 | 2020-02-14 | 四川正蓉实业有限公司 | Modified composite barite for drilling fluid |
| CN111349350A (en) * | 2020-03-13 | 2020-06-30 | 大连环球矿产股份有限公司 | Inorganic composite powder and preparation method thereof |
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| CN112210232A (en) * | 2020-08-24 | 2021-01-12 | 江西广源化工有限责任公司 | Special superfine heavy calcium carbonate for latex gloves and preparation method and application thereof |
| CN112521685A (en) * | 2020-11-23 | 2021-03-19 | 江苏金发科技新材料有限公司 | Hydrophobic polyolefin composition and preparation method thereof |
| CN112745701A (en) * | 2020-12-18 | 2021-05-04 | 广西碳酸钙产业化工程院有限公司 | Modified heavy calcium powder, super-hydrophobic coating prepared from modified heavy calcium powder, preparation method, use method and application of super-hydrophobic coating |
| CN112812587A (en) * | 2021-01-08 | 2021-05-18 | 深圳市锦昊辉实业发展有限公司 | Active nano calcium, preparation method thereof and application thereof in preparation of silicone sealant |
| CN112940537A (en) * | 2021-01-29 | 2021-06-11 | 广西碳酸钙产业化工程院有限公司 | Special heavy calcium carbonate for coating and preparation method thereof |
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