CN106366696A - Preparation method of active calcium carbonate used for foaming ethylene-vinyl acetate copolymer - Google Patents
Preparation method of active calcium carbonate used for foaming ethylene-vinyl acetate copolymer Download PDFInfo
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- CN106366696A CN106366696A CN201610695908.8A CN201610695908A CN106366696A CN 106366696 A CN106366696 A CN 106366696A CN 201610695908 A CN201610695908 A CN 201610695908A CN 106366696 A CN106366696 A CN 106366696A
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- calcium carbonate
- vinyl acetate
- acetate copolymer
- ethylene
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- 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
-
- 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
-
- 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
- C09C3/10—Treatment with macromolecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
Abstract
The invention provides a preparation method of active calcium carbonate used for foaming ethylene-vinyl acetate copolymer. The active calcium carbonate can improve the dispersibility and the stability of a filler and improve the compatibility between the filler and ethylene-vinyl acetate copolymer resin. The preparation method concretely comprises the following steps: 1, adding 400-600 mesh calcium carbonate powder to water, a hyper-dispersant and an anti-precipitating agent to prepare a slurry with the solid content of 60-80%; 2, adding the slurry obtained in step 1 into a vertical stirring wet grinding machine, and carrying out wet grinding under certain conditions; 3, putting the slurry obtained in step 2in a vibrating sieve to obtain a slurry with the content fraction of particles with the fineness of 1 [mu]m or less being higher than 90%; 5, carrying out flash evaporation drying on the slurry obtained in step 3, and adding ethylene-vinyl acetate copolymer wax in the drying process in order to carry out surface coating treatment; an 5, carrying out grading collection.
Description
[technical field]
The present invention relates to ground calcium carbonate field of deep, more particularly, to a kind of ethylene-vinyl acetate copolymer foamed use
The preparation method of activated Calcium carbonate.
[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 is mainly used in the industries such as rubber, plastics, papermaking, coating, and its usage amount exceedes
The precipitated calcium carbonate being produced by chemical method.
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).The production method of superfine heavy calcium carbonate mainly has two kinds of dry and wet, dry production
Superfine heavy calcium carbonate fineness can reach 3000 mesh；It is all mainly to produce using wet grinding to surpass more than the product of 3000 mesh
Thin ground calcium carbonate.
In ethylene-vinyl acetate copolymer (also referred to as ethene-vinyl acetate copolymer, ethylene vinyl
Acetate, abbreviation eva) foaming shoe material field, the filler that tradition uses is lightweight nm-class active calcium carbonate.Traditional lightweight is received
Rice activated Calcium carbonate adopts chemical precipitation method to produce, and the technological process of production is complicated, and environmental pollution is larger, and chemical property is unstable
Fixed；In process of production, using stearic acid as surfactant, but because stearic fusing point is relatively low, easily produce yellow
Become, bad with the binding ability of ethylene-vinyl acetate copolymer base material it is impossible to meet the demand in present market.
[content of the invention]
For drawbacks described above of the prior art, the present invention provides a kind of ethylene-vinyl acetate copolymer foamed activity
The preparation method of Calcium Carbonate, it is possible to increase the dispersibility of filler and stability, improves filler and ethylene-vinyl acetate copolymer tree
The compatibility of fat.
The technical scheme is that
A kind of preparation method of ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate is it is characterised in that include following
Step:
(1) calcium carbonate powder of 400-600 mesh is added water, hyper-dispersant and antiprecipitant, being configured to solid content is
The slurry of 60-80%；
(2) slurry that step (1) obtains is put into vertical mixing wet grinding mill, carry out wet method under certain conditions and grind
Mill；
(3) vibrosieve put into by the slurry obtaining step (2), obtains the running summary of the points scored that fineness is less than 1 μm granule
Slurry higher than 90%；
(4) slurry that (3) after step obtain is carried out expansion drying, add ethene-vinyl acetate during drying
Copolymer waxes carry out Surface coating process；
(5) classification is collected.The Paris white being surface-treated is classified, is collected the product of more than 6000 mesh.
This technical scheme passes through the super fine powder processing technique of dry grinding and wet grinding, can grind powder granule
To 6000 mesh, at 1-1.5 μm, bet specific surface area is more than 20m to its mean diameter2/g.The size of powder granule and fabricated product
Surface gloss has great relation, and powder granule is thinner, and its surface gloss is higher；Using ethene-vinyl acetate copolymerization
The modified technique of thing wax, is surface-treated in expansion drying simultaneously, and the activation grade of product surface is more than 98%, powder body material
Surface active degree is higher, and its hydrophobicity is stronger, and its oil absorption is also stronger accordingly, also stronger with the associativity of substrate resin；Adopt
With ethylene-vinyl acetate copolymer wax as surface capping agents, the compatibility with ethylene-vinyl acetate copolymer resin is high, carries
The high associativity with ethylene-vinyl acetate copolymer base material, effectively solves ethylene-vinyl acetate copolymer foamed footwear material
Add the problem that the tear resistance after filler declines in material, improve tearing toughness.
Further, the calcium carbonate powder of above-mentioned 400-600 mesh is obtained by following steps: calcite is carried out, sieves
Select, be crushed to the calcium carbonate granule of 1-3cm, then carry out dry grinding, be classified by fineness using cyclone classified system, collect
The calcium carbonate powder of 400-600 mesh.
Further, above-mentioned hyper-dispersant is water-soluble sodium polyacrylate salt.
Further, the addition of above-mentioned hyper-dispersant is the 5-15 ‰ of calcite quality.
Further, above-mentioned antiprecipitant is sodium naphthalene sulfonate antiprecipitant.
Further, the addition of above-mentioned antiprecipitant accounts for the 1-8 ‰ of calcite in powder weight.
Further, the rotating speed of above-mentioned steps (2) wet grinding is 2500r/min, and grinding temperature is 80 DEG C, abrasive media
Zirconium oxide microballon for diameter 2-5mm.
Further, the addition of above-mentioned ethylene-vinyl acetate copolymer wax is the 0.5-2% of Calcium Carbonate quality.
The present invention has following beneficial technique effect: the present invention carries out surface using ethylene-vinyl acetate copolymer wax
Cladding processes Calcium Carbonate, and its surface coating rate may be up to 98%；Ethylene-vinyl acetate copolymer wax conduct of the present invention
Surface capping agents, the compatibility with ethylene-vinyl acetate copolymer resin is high, improves and ethylene-vinyl acetate copolymer base
The associativity of material；Hyper-dispersant and antiprecipitant that the present invention adds during preparing slurry, effectively raise slurry
Dispersibility and suspension, be that the stability of subsequent wet abrasive product provides guarantee；The present invention can realize calcium carbonate wet
Fineness after method is ground reaches 6000 mesh, improves its specific surface area and reaches 20m2/g；Technique of the present invention is total enclosing
The physical grinding process of formula, no any environmental pollution, environmental protection and energy saving.
[brief description]
Fig. 1 is the flow chart of steps 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
Industrial raw ore calcite is carried out, screens, being crushed to the calcium carbonate granule of 1-3cm, by grinding using ring roll
Carry out dry grinding, carry out being classified, collect prepared 400 mesh coarse powder by cyclone classified system；Being configured to solid content with water again is
75% slurry, adds the water solublity hyper-dispersant polyacrylic acid sodium salt of powder quality 0.8% and 0.1% antisolvent precipitation simultaneously
Agent；Then slurry input vertical wet-process agitator mill is carried out constant temperature wet grinding, grinding temperature is 80 DEG C, abrasive media is oxygen
Change zirconium microballon, obtain 6000 mesh slurries and cross vibrosieve, obtain the slurry that the running summary of the points scored that fineness is less than 1 μm granule is higher than 90%
Material；Slurry is pumped into rapid flash be dried, add ethylene-vinyl acetate copolymer wax simultaneously and carry out Surface coating process, add
Measure 0.5% for Calcium Carbonate quality；Particle classifying is collected after terminating by modification, ethyl vinyl acetate is obtained through automatic packaging machine packaging
Ethylene copolymer foaming special active Calcium Carbonate.
Embodiment two
Industrial raw ore calcite is carried out, screens, being crushed to the calcium carbonate granule of 1-3cm, by grinding using ring roll
Carry out dry grinding, carry out being classified, collect prepared 500 mesh coarse powder by cyclone classified system；Being configured to solid content with water again is
60% slurry, adds the water solublity hyper-dispersant polyacrylic acid sodium salt of powder quality 1% and 0.3% antiprecipitant simultaneously；
Then slurry input vertical wet-process agitator mill is carried out constant temperature wet grinding, grinding temperature is 80 DEG C, abrasive media is oxidation
Zirconium microballon, obtains 6000 mesh slurries and crosses vibrosieve, obtains the slurry that the running summary of the points scored that fineness is less than 1 μm granule is higher than 90%；
Slurry is pumped into rapid flash be dried, add ethylene-vinyl acetate copolymer wax simultaneously and carry out Surface coating process, addition is
The 0.8% of Calcium Carbonate quality；Particle classifying is collected after terminating by modification, ethene-vinyl acetate is obtained through automatic packaging machine packaging
Co-polymer foamed special active Calcium Carbonate.
Embodiment three
Industrial raw ore calcite is carried out, screens, being crushed to the calcium carbonate granule of 1-3cm, by grinding using ring roll
Carry out dry grinding, carry out being classified, collect prepared 600 mesh coarse powder by cyclone classified system；Being configured to solid content with water again is
80% slurry, adds the water solublity hyper-dispersant polyacrylic acid sodium salt of powder quality 1% and 0.5% antiprecipitant simultaneously；
Then slurry input vertical wet-process agitator mill is carried out constant temperature wet grinding, grinding temperature is 80 DEG C, abrasive media is oxidation
Zirconium microballon, obtains 6000 mesh slurries and crosses vibrosieve, obtains the slurry that the running summary of the points scored that fineness is less than 1 μm granule is higher than 90%；
Slurry is pumped into rapid flash be dried, add ethylene-vinyl acetate copolymer wax simultaneously and carry out Surface coating process, addition is
The 0.5% of Calcium Carbonate quality；Particle classifying is collected after terminating by modification, ethene-vinyl acetate is obtained through automatic packaging machine packaging
Co-polymer foamed special active Calcium Carbonate.
Example IV
Industrial raw ore calcite is carried out, screens, being crushed to the calcium carbonate granule of 1-3cm, by grinding using ring roll
Carry out dry grinding, carry out being classified, collect prepared 400 mesh coarse powder by cyclone classified system；Being configured to solid content with water again is
75% slurry, adds the water solublity hyper-dispersant polyacrylic acid sodium salt of powder quality 1.5% and 0.8% antisolvent precipitation simultaneously
Agent；Then slurry input vertical wet-process agitator mill is carried out constant temperature wet grinding, grinding temperature is 80 DEG C, abrasive media is oxygen
Change zirconium microballon, obtain 6000 mesh slurries and cross vibrosieve, obtain the slurry that the running summary of the points scored that fineness is less than 1 μm granule is higher than 90%
Material；Slurry is pumped into rapid flash be dried, add ethylene-vinyl acetate copolymer wax simultaneously and carry out Surface coating process, add
Measure 1.5% for Calcium Carbonate quality；Particle classifying is collected after terminating by modification, ethyl vinyl acetate is obtained through automatic packaging machine packaging
Ethylene copolymer foaming special active Calcium Carbonate.
Embodiment five
Industrial raw ore calcite is carried out, screens, being crushed to the calcium carbonate granule of 1-3cm, by grinding using ring roll
Carry out dry grinding, carry out being classified, collect prepared 400 mesh coarse powder by cyclone classified system；Being configured to solid content with water again is
75% slurry, adds the water solublity hyper-dispersant polyacrylic acid sodium salt of powder quality 1.5% and 1.0% antisolvent precipitation simultaneously
Agent；Then slurry input vertical wet-process agitator mill is carried out constant temperature wet grinding, grinding temperature is 80 DEG C, abrasive media is oxygen
Change zirconium microballon, obtain 6000 mesh slurries and cross vibrosieve, obtain the slurry that the running summary of the points scored that fineness is less than 1 μm granule is higher than 90%
Material；Slurry is pumped into rapid flash be dried, add ethylene-vinyl acetate copolymer wax simultaneously and carry out Surface coating process, add
Measure 2% for Calcium Carbonate quality；Particle classifying is collected after terminating by modification, ethyl vinyl acetate second is obtained through automatic packaging machine packaging
Alkene copolymer foaming special active Calcium Carbonate.
The testing result of the product of above example one to five see table:
Claims (8)
1. a kind of preparation method of ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate is it is characterised in that include following walking
Rapid:
(1) calcium carbonate powder of 400-600 mesh is added water, hyper-dispersant and antiprecipitant, being configured to solid content is 60-80%
Slurry；
(2) slurry that step (1) obtains is put into vertical mixing wet grinding mill and carry out wet grinding；
(3) vibrosieve put into by the slurry obtaining step (2), and obtaining the running summary of the points scored that fineness is less than 1 μm granule is higher than 90%
Slurry；
(4) slurry that (3) after step obtain is carried out expansion drying, add ethene-vinyl acetate copolymerization during drying
Thing wax carries out Surface coating process；
(5) classification is collected.The Paris white being surface-treated is classified, is collected the product of more than 6000 mesh.
2. the preparation method of ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate according to claim 1, its feature
It is, the calcium carbonate powder of described 400-600 mesh is obtained by following steps: calcite is carried out, screens, is crushed to 1-
The calcium carbonate granule of 3cm, then carry out dry grinding, it is classified by fineness using cyclone classified system, collected 400-600 purpose
Calcium carbonate powder.
3. the preparation method of ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate according to claim 1, its feature
It is, described hyper-dispersant is water-soluble sodium polyacrylate salt.
4. the preparation method of the ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate according to claim 1 or 3, its
It is characterised by, the addition of described hyper-dispersant is the 5-15 ‰ of calcite quality.
5. the preparation method of ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate according to claim 1, its feature
It is, described antiprecipitant is sodium naphthalene sulfonate antiprecipitant.
6. the preparation method of ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate according to claim 1 or 5, its
It is characterised by, the addition of described antiprecipitant accounts for the 1-8 ‰ of calcite in powder weight.
7. the preparation method of ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate according to claim 1, its feature
It is, the rotating speed of described step (2) wet grinding is 2500r/min, and grinding temperature is 80 DEG C, and abrasive media is diameter 2-5mm
Zirconium oxide microballon.
8. the preparation method of ethylene-vinyl acetate copolymer foamed use activated Calcium carbonate according to claim 1, its feature
It is, the addition of described ethylene-vinyl acetate copolymer wax is the 0.5-2% of Calcium Carbonate quality.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610695908.8A CN106366696A (en) | 2016-08-22 | 2016-08-22 | Preparation method of active calcium carbonate used for foaming ethylene-vinyl acetate copolymer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111670070A (en) * | 2017-11-17 | 2020-09-15 | 因可亚合伙人有限责任公司 | Method for preparing a composition comprising untreated and surface-treated alkaline earth metal carbonates and the composition |
| CN114716848A (en) * | 2022-04-29 | 2022-07-08 | 江西广源化工有限责任公司 | Superfine heavy calcium carbonate and preparation method and application thereof |
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2016
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111670070A (en) * | 2017-11-17 | 2020-09-15 | 因可亚合伙人有限责任公司 | Method for preparing a composition comprising untreated and surface-treated alkaline earth metal carbonates and the composition |
| CN114716848A (en) * | 2022-04-29 | 2022-07-08 | 江西广源化工有限责任公司 | Superfine heavy calcium carbonate and preparation method and application thereof |
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