CN105820601B - A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink - Google Patents
A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink Download PDFInfo
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- CN105820601B CN105820601B CN201610247624.2A CN201610247624A CN105820601B CN 105820601 B CN105820601 B CN 105820601B CN 201610247624 A CN201610247624 A CN 201610247624A CN 105820601 B CN105820601 B CN 105820601B
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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
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
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- 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
- C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
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- 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
- C09C3/043—Drying, calcination
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- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention provides a kind of preparation of high-grade Nano calcium carbonate dedicated to printing ink, includes the following steps：（1）Milk of lime is diluted, proportion is adjusted, is then delivered to carbonation reaction tower；（2）Purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry；（3）Ripe slurry is delivered to surface treatment tank, surface conditioning agent is added and is surface-treated, modified nano calcium carbonate is obtained；（4）Modified nano calcium carbonate is subjected to filter-press dehydration, dry, pulverize, be classified, pack to get to the present invention high-grade Nano calcium carbonate dedicated to printing ink；The surface conditioning agent is the saponification liquor of linoleic acid and maleic acid.The high-grade Nano calcium carbonate dedicated to printing ink that the present invention obtains is filled applied to gravure ink, has mobility high, and transparency is good, and drying time is short, and without gelatinization phenomenon after heating, fluidity variation is small, the advantage that product quality is stablized.
Description
Technical field
The present invention relates to a kind of preparations of nano-calcium carbonate, and in particular to a kind of system of top grade Nano calcium carbonate dedicated to printing ink
It is standby.
Background technology
Printing ink producing enterprise of China has more than 180 families, about 500,000 tons of annual output to account for about the 7% of world's ink yield, at present
As the fourth-largest Printing ink producing state of the world.The development of press and ink industry has driven the development of ink calcium carbonate for special use.Nanometer
Calcium carbonate shows excellent dispersibility, the transparency as printing ink filler in ink system, has and covers well
Power, alternative titanium dioxide reduce Printing ink producing cost.
Ink type is various, and different types of ink, different Printing ink producing producers are to the properties of nano-calcium carbonate
There is different requirements.Commercial inks use nano-calcium carbonate to mostly use resin acid and fatty acid complex to match as surface conditioning agent.Resin
Acid is preferable with the link stuff compatibility of ink, and calcium carbonate can be made to obtain preferable dispersibility and the transparency.However resin acid is but
The drying being unfavorable for after ink printing, and its thermal stability is often poor, is easy oxidation deterioration.In addition, calcium carbonate belongs to alkalinity
Filler, pH control the improper gelatinization, retrogradation and caking that can cause ink.These factors limit nano-calcium carbonate in ink
Using.
1916084 A of Chinese invention patent CN disclose a kind of preparation method of Nano calcium carbonate dedicated to printing ink.This method
Crystal control agent and dispersant is added at 15~40 DEG C in the initial temperature that is carbonized control in carbonisation, tree is added after reaction
Resin acid and its derivative are surface-treated nano-calcium carbonate.Although can get by nano-calcium carbonate prepared by the invention preferable
Dispersibility and the transparency, but be unfavorable for the quick-drying of ink, and the outstanding problems such as ink gelatinization and caking cannot be solved.
1634767 A of Chinese invention patent CN disclose a kind of manufacturing method of ink nano-calcium carbonate.This method exists
A certain amount of nucleus is added before carbonating and forms accelerating agent, is carried out using hydroabietic acid or disproportionated rosin acid after carbonating
Surface is modified.Although hydrogenated rosin and disproportionated rosin can improve the heat-resistant stability of rosin acid, ink to a certain extent
Rate of drying be greatly affected.
In conclusion the technology of preparing of disclosed ink nano-calcium carbonate is difficult to meet higher standard ink at present
Filling demand.
Invention content
The object of the present invention is to provide a kind of preparation of high-grade Nano calcium carbonate dedicated to printing ink, the height that this method obtains
It is basic that shelves Nano calcium carbonate dedicated to printing ink can not only meet dispersibility, the transparency, the high photosensitiveness of filler in ink system etc.
It is required that and the quick-drying of ink can be effectively improved, solve the difficulties such as ink gelatinization, caking, retrogradation for being caused by alkaline filler
Topic.
To achieve the goals above, the technical solution adopted by the present invention is as follows：
The present invention is control carbonating technique appropriate, the nano-calcium carbonate of specific surface area 20-35 ㎡/g is prepared, using Asia
Linolenic acid and maleic acid compounding are surface-treated.The link stuff of linoleic acid and ink has preferable compatible
Property, and the rate of drying of ink is not interfered with, while maleic acid has higher acid value, can effectively inhibit ink
Gelatinization and caking are conducive to stablizing for ink system and preserve.
A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, includes the following steps：
(1) refined, 36~72h of ageing milk of lime is diluted, proportion is adjusted to 1.050~1.065, is then delivered to
Carbonation reaction tower, initial temperature are 18~23 DEG C；
(2) will purification, kiln gas after cooling be passed through carbonation reaction tower carry out carbonation reaction, kiln gas flow be 2~
5m3/ h, carbon dioxide volume content are 30~35%, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, ripe slurry compares table
Area is 20~35m2/g；
(3) the ripe slurry that step (2) obtains is delivered to surface treatment tank, is heated to 65~90 DEG C, surface conditioning agent is added
It is surface-treated, 30~60min of high-speed stirred obtains modified nano calcium carbonate；
(4) modified nano calcium carbonate for obtaining step (3) carries out filter-press dehydration, is dried by chain belt drying machine, dry
Temperature be 100~110 DEG C, using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
The surface conditioning agent is the saponification liquor of linoleic acid and maleic acid；Wherein linoleic acid and suitable fourth
The weight ratio of enedioic acid is 1~3:1.
The addition of surface conditioning agent linoleic acid and maleic acid described above is that nano-calcium carbonate is dry in ripe slurry
The 3.0~4.5% of matrix amount.
The preparation method of surface conditioning agent described above is will to state linoleic acid and maleic acid soap occurs with highly basic
Change the obtained water-soluble saponification liquor of reaction；Wherein the temperature of saponification is 90 DEG C, and highly basic dosage is linoleic acid and maleic
The 5~10% of diacid total amount.
Highly basic described above is sodium hydroxide or potassium hydroxide.
The rotating speed of high-speed stirred described above is 800-1500r/min.
Advantageous effect
1, high-grade Nano calcium carbonate dedicated to printing ink pH value of the invention has good between 8.5~9.0 in ink system
Good dispersibility, mobility and high transparency can be effectively improved the quick-drying of ink, solve ink easy glue in Storage period
The problems such as change, caking, retrogradation, has wide application market in ink area.
2, present invention process is simple, and production cost is low, industrialized production easy to implement, has good economic benefit and society
Benefit.
3, gravure ink made of high-grade Nano calcium carbonate dedicated to printing ink of the invention, with conventional modified nano calcium carbonate phase
Than having mobility high, transparency is good, and drying time is short, and without gelatinization phenomenon after heating, fluidity variation is small, stable quality
The advantages of.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 modified nano calcium carbonate product of embodiment, and grain size is about 65nm, cubic, homogeneity
It is good.
Specific implementation mode
One, embodiment is prepared
Embodiment 1
A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, includes the following steps：
(1) refined, ageing 36h milk of lime is diluted, proportion is adjusted to 1.050, is then delivered to carbonation reaction
Tower, initial temperature are 18 DEG C；
(2) purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, kiln gas flow is 2m3/ h,
Carbon dioxide volume content is 30%, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, and ripe slurry specific surface area is 20m2/
g；
(3) the ripe slurry that step (2) obtains is delivered to surface treatment tank, is heated to 65 DEG C, surface conditioning agent is added and carries out
Surface treatment, the wherein addition of surface conditioning agent linoleic acid and maleic acid are nano-calcium carbonate butt matter in ripe slurry
The 3.0% of amount, adjustment rotating speed are 800r/min, stir 30min, obtain modified nano calcium carbonate；
(4) modified nano calcium carbonate for obtaining step (3) carries out filter-press dehydration, is dried by chain belt drying machine, dry
Temperature be 100 DEG C, using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
Surface conditioning agent described in the present embodiment is that under sodium hydroxide effect soap occurs for linoleic acid and maleic acid
Change the water-soluble saponification liquor of reaction gained.Wherein the weight ratio of linoleic acid and maleic acid is 1:1, saponification temperature 90
DEG C, sodium hydroxide concentration is the 5% of linoleic acid and maleic acid total amount.
Embodiment 2
A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, includes the following steps：
(1) refined, ageing 72h milk of lime is diluted, proportion is adjusted to 1.065, is then delivered to carbonation reaction
Tower, initial temperature are 23 DEG C；
(2) purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, kiln gas flow is 5m3/ h,
Carbon dioxide volume content is 35%, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, and ripe slurry specific surface area is 35m2/
g；
(3) the ripe slurry that step (2) obtains is delivered to surface treatment tank, is heated to 90 DEG C, surface conditioning agent is added and carries out
Surface treatment, the wherein addition of surface conditioning agent linoleic acid and maleic acid are nano-calcium carbonate butt matter in ripe slurry
The 4.5% of amount, adjustment rotating speed are 1200r/min, stir 60min, obtain modified nano calcium carbonate；
(4) modified nano calcium carbonate for obtaining step (3) carries out filter-press dehydration, is dried by chain belt drying machine, dry
Temperature be 110 DEG C, using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
Surface conditioning agent described in the present embodiment is that under potassium hydroxide effect soap occurs for linoleic acid and maleic acid
Change the water-soluble saponification liquor of reaction gained.Wherein the weight ratio of linoleic acid and maleic acid is 3:1, saponification temperature 90
DEG C, potassium hydroxide dosage is the 10% of linoleic acid and maleic acid total amount.
Embodiment 3
A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, includes the following steps：
(1) refined, ageing 48h milk of lime is diluted, proportion is adjusted to 1.055, is then delivered to carbonation reaction
Tower, initial temperature are 21 DEG C；
(2) purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, kiln gas flow is 3m3/ h,
Carbon dioxide volume content is 33%, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, ripe slurry specific surface area is
27.8m2/g；
(3) the ripe slurry that step (2) obtains is delivered to surface treatment tank, is heated to 75 DEG C, surface conditioning agent is added and carries out
Surface treatment, the wherein addition of surface conditioning agent linoleic acid and maleic acid are nano-calcium carbonate butt matter in ripe slurry
The 4% of amount, adjustment rotating speed are 1500r/min, stir 45min, obtain modified nano calcium carbonate；
(4) modified nano calcium carbonate for obtaining step (3) carries out filter-press dehydration, is dried by chain belt drying machine, dry
Temperature be 105 DEG C, using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
Surface conditioning agent described in the present embodiment is that under sodium hydroxide effect soap occurs for linoleic acid and maleic acid
Change the water-soluble saponification liquor of reaction gained.Wherein the weight ratio of linoleic acid and maleic acid is 2:1, saponification temperature 90
DEG C, sodium hydroxide concentration is the 7% of linoleic acid and maleic acid total amount.
Embodiment 4
A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, includes the following steps：
(1) refined, ageing 48h milk of lime is diluted, proportion is adjusted to 1.060, is then delivered to carbonation reaction
Tower, initial temperature are 19 DEG C；
(2) purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, kiln gas flow is 4m3/ h,
Carbon dioxide volume content is 32%, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, ripe slurry specific surface area is
26.4m2/g；
(3) the ripe slurry that step (2) obtains is delivered to surface treatment tank, is heated to 80 DEG C, surface conditioning agent is added and carries out
Surface treatment, the wherein addition of surface conditioning agent linoleic acid and maleic acid are nano-calcium carbonate butt matter in ripe slurry
The 3.5% of amount, adjustment rotating speed are 1200r/min, stir 40min, obtain modified nano calcium carbonate；
(4) modified nano calcium carbonate for obtaining step (3) carries out filter-press dehydration, is dried by chain belt drying machine, dry
Temperature be 105 DEG C, using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
Surface conditioning agent described in the present embodiment is that under potassium hydroxide effect soap occurs for linoleic acid and maleic acid
Change the water-soluble saponification liquor of reaction gained.Wherein the weight ratio of linoleic acid and maleic acid is 2:1, saponification temperature 90
DEG C, potassium hydroxide dosage is the 8% of linoleic acid and maleic acid total amount.
Embodiment 5
A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, includes the following steps：
(1) refined, ageing 48h milk of lime is diluted, proportion is adjusted to 1.060, is then delivered to carbonation reaction
Tower, initial temperature are 21 DEG C；
(2) purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, kiln gas flow is 3m3/ h,
Carbon dioxide volume content is 34%, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, ripe slurry specific surface area is
29.0m2/g；
(3) the ripe slurry that step (2) obtains is delivered to surface treatment tank, is heated to 85 DEG C, surface conditioning agent is added and carries out
Surface treatment, the wherein addition of surface conditioning agent linoleic acid and maleic acid are nano-calcium carbonate butt matter in ripe slurry
The 4% of amount, adjustment rotating speed are 1000r/min, stir 50min, obtain modified nano calcium carbonate；
(4) modified nano calcium carbonate for obtaining step (3) carries out filter-press dehydration, is dried by chain belt drying machine, dry
Temperature be 105 DEG C, using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
Surface conditioning agent described in the present embodiment is that under potassium hydroxide effect soap occurs for linoleic acid and maleic acid
Change the water-soluble saponification liquor of reaction gained.Wherein the weight ratio of linoleic acid and maleic acid is 3:1, saponification temperature 90
DEG C, potassium hydroxide dosage is the 6% of linoleic acid and maleic acid total amount.
Embodiment 6
A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, includes the following steps：
(1) refined, ageing 48h milk of lime is diluted, proportion is adjusted to 1.055, is then delivered to carbonation reaction
Tower, initial temperature are 20 DEG C；
(2) purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, kiln gas flow is 3m3/ h,
Carbon dioxide volume content is 33%, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, ripe slurry specific surface area is
32.6m2/g；
(3) the ripe slurry that step (2) obtains is delivered to surface treatment tank, is heated to 80 DEG C, surface conditioning agent is added and carries out
Surface treatment, the wherein addition of surface conditioning agent linoleic acid and maleic acid are nano-calcium carbonate butt matter in ripe slurry
The 4.5% of amount, adjustment rotating speed are 1500r/min, stir 35min, obtain modified nano calcium carbonate；
(4) modified nano calcium carbonate for obtaining step (3) carries out filter-press dehydration, is dried by chain belt drying machine, dry
Temperature be 105 DEG C, using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
Surface conditioning agent described in the present embodiment is that under potassium hydroxide effect soap occurs for linoleic acid and maleic acid
Change the water-soluble saponification liquor of reaction gained.Wherein the weight ratio of linoleic acid and maleic acid is 1:1, saponification temperature 90
DEG C, potassium hydroxide dosage is the 5% of linoleic acid and maleic acid total amount.
Two, comparative example
Comparative example 1
Refined, ageing 48h milk of lime is diluted, proportion is adjusted to 1.060, is then delivered to carbonating column；Initially
Temperature is 19 DEG C；It is passed through purification, kiln gas after cooling progress carbonation reaction, kiln gas flow is 4m3/ h, carbon dioxide volume contain
Amount is 32%, when reaction solution pH drops to 7.0, obtains ripe slurry, ripe slurry specific surface area test is 26.4m2/g；Ripe slurry is delivered to
Be surface-treated pond, temperature is heated to 80 DEG C, is added the saponification liquor of 3.5% rosin acid and stearic acid compounding, wherein rosin acid with it is hard
The proportioning of resin acid is 2:1, sodium hydroxide concentration is the 14% of the two total amount；High-speed stirred 40min completes surface and is modified；It will processing
Good slurry carries out filter-press dehydration, and processing is dried by chain belt drying machine, and drying temperature is 105 DEG C, is finally crushed, point
Grade, packaging is to get to the nano-calcium carbonate sample used in this comparative example 1.
Comparative example 2
Refined, ageing 48h milk of lime is diluted, proportion is adjusted to 1.060, is then delivered to carbonating column；Initially
Temperature is 21 DEG C；It is passed through purification, kiln gas after cooling progress carbonation reaction, kiln gas flow is 3m3/ h, carbon dioxide volume contain
Amount is 34%, when reaction solution pH drops to 7.0, obtains ripe slurry, ripe slurry specific surface area test is 29.0m2/g；Ripe slurry is delivered to
Surface treatment pond, temperature are heated to 85 DEG C, and the saponification liquor of 4% rosin acid and stearic acid compounding, wherein rosin acid and tristearin is added
The proportioning of acid is 3:1, sodium hydroxide concentration is the 14% of the two total amount；High-speed stirred 50min completes surface and is modified；It will handle well
Slurry carry out filter-press dehydration, be dried processing by chain belt drying machine, drying temperature is 105 DEG C, is finally crushed, classification,
Packaging is to get to the nano-calcium carbonate sample used in this comparative example 2.
Three, comparative analysis
The nano-calcium carbonate that various embodiments of the present invention and comparative example obtain is formulated according to a conventional method as shown in table 1
Prepare gravure ink.Each embodiment and gravure ink performance obtained by comparative example are as shown in table 2.
Table 1：Prepare gravure ink formula
| Raw material | Weight percent (%) |
| Phthalocyanine blue | 10.0 |
| Resin plasticizer | 2.5 |
| Nano-calcium carbonate | 12 |
| Wax | 7.5 |
| Chlorinated rubber | 12 |
| Toluene | 38 |
| Phenol-formaldehyde resin modified | 18 |
Table 2：Gravure ink the performance test results
The above performance fluidity test method is with reference to GB/T 14624.3-93；Ink stability test method is with reference to QB
567-83；The method of inspection of ink dryness is with reference to QB 562-83；The method of inspection of the ink transparency is with reference to GB/T 14624.1-
93。
It can be seen from the above, gravure ink made of high-grade Nano calcium carbonate dedicated to printing ink, with conventional modified nano calcium carbonate
It compares, mobility is high, and transparency is good, and drying time is short, stablizes without gelatinization phenomenon, product quality after heating.
Claims (2)
1. a kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, which is characterized in that include the following steps：
（1）Refined, 36~72h of ageing milk of lime is diluted, proportion is adjusted to 1.050~1.065, is then delivered to carbonic acid
Change reaction tower, initial temperature is 18~23 DEG C；
（2）Purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, kiln gas flow is 2~5m3/h,
Carbon dioxide volume content is 30~35%, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, and ripe slurry specific surface area is 20
~35m2/g；
（3）By step（2）Obtained ripe slurry is delivered to surface treatment tank, is heated to 65~90 DEG C, and surface conditioning agent is added and carries out
Surface treatment, 30~60min of high-speed stirred obtain modified nano calcium carbonate；
（4）By step（3）Obtained modified nano calcium carbonate carries out filter-press dehydration, is dried by chain belt drying machine, dry temperature
Degree is 100~110 DEG C, and using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
The surface conditioning agent is the saponification liquor of linoleic acid and maleic acid；Wherein linoleic acid and maleic two
The weight ratio of acid is 1~3:1；
The addition of the surface conditioning agent linoleic acid and maleic acid is nano-calcium carbonate butt quality in ripe slurry
3.0~4.5%；
The rotating speed of the high-speed stirred is 800-1500r/min；
The preparation method of the surface conditioning agent is will to state linoleic acid and maleic acid saponification institute occurs with highly basic
Obtained water-soluble saponification liquor；Wherein the temperature of saponification is 90 DEG C, and highly basic dosage is linoleic acid and maleic acid total amount
5~10%；
The highly basic is sodium hydroxide or potassium hydroxide.
2. a kind of preparation of top grade Nano calcium carbonate dedicated to printing ink, includes the following steps：
（1）Refined, ageing 36h milk of lime is diluted, proportion is adjusted to 1.050, is then delivered to carbonation reaction tower, just
Beginning temperature is 18 DEG C；
（2）Purification, kiln gas after cooling are passed through carbonation reaction tower and carry out carbonation reaction, kiln gas flow is 2m3/h, dioxy
It is 30% to change carbon volume content, and reaction is terminated when reaction solution pH drops to 7.0, obtains ripe slurry, and ripe slurry specific surface area is 20m2/g；
（3）By step（2）Obtained ripe slurry is delivered to surface treatment tank, is heated to 65 DEG C, and surface conditioning agent is added and carries out surface
Processing, the wherein addition of surface conditioning agent linoleic acid and maleic acid are nano-calcium carbonate butt quality in ripe slurry
3.0%, adjustment rotating speed is 800r/min, stirs 30min, obtains modified nano calcium carbonate；
（4）By step（3）Obtained modified nano calcium carbonate carries out filter-press dehydration, is dried by chain belt drying machine, dry temperature
Degree is 100 DEG C, and using crushing, classification, packaging is to get to high-grade Nano calcium carbonate dedicated to printing ink；
The surface conditioning agent is that linoleic acid and maleic acid occur under sodium hydroxide effect obtained by saponification
Water-soluble saponification liquor；Wherein the weight ratio of linoleic acid and maleic acid is 1:1, saponification temperature is 90 DEG C, sodium hydroxide
Dosage is the 5% of linoleic acid and maleic acid total amount.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610247624.2A CN105820601B (en) | 2016-04-18 | 2016-04-18 | A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610247624.2A CN105820601B (en) | 2016-04-18 | 2016-04-18 | A kind of preparation of top grade Nano calcium carbonate dedicated to printing ink |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105820601A CN105820601A (en) | 2016-08-03 |
| CN105820601B true CN105820601B (en) | 2018-09-14 |
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| CN106673043B (en) * | 2017-01-06 | 2017-11-14 | 河北立信化工有限公司 | Polyethersulfone resin filling anti-oxidant nano-calcium carbonate of toughness reinforcing uvioresistant and its production and use |
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| EP1557442A1 (en) * | 2004-01-23 | 2005-07-27 | SOLVAY (Société Anonyme) | Method for surface treatment of precipitated calcium carbonate |
| EP2537806B1 (en) * | 2010-02-15 | 2019-12-04 | Shiraishi Kogyo Kaisha, Ltd. | Surface-treated calcium carbonate and paste-like resin composition containing same |
| CN103665937B (en) * | 2013-11-28 | 2015-07-01 | 广西华纳新材料科技有限公司 | Method for preparing nano calcium carbonate specially used for middle and top grade silicone sealants |
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