CN1916084A - Method for preparing Nano calcium carbonate dedicated to printing ink - Google Patents
Method for preparing Nano calcium carbonate dedicated to printing ink Download PDFInfo
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- CN1916084A CN1916084A CN 200510112374 CN200510112374A CN1916084A CN 1916084 A CN1916084 A CN 1916084A CN 200510112374 CN200510112374 CN 200510112374 CN 200510112374 A CN200510112374 A CN 200510112374A CN 1916084 A CN1916084 A CN 1916084A
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Abstract
This invention discloses a method for preparing special nanoscale calcium carbonate for ink. The method comprises: calcining natural calcium carbonate, slaking, carbonzing, coating by a coating agent, vacuum-filtering and drying to obtain nanoscale calcium carbonate. The initial carbonization temperature is 15-40 deg.C, and crystal-morphology regulator and dispersant are added during carbonization. The coating agent is resinic acid and its derivatives. The obtained nanoscale calcium carbonate has such advantages as high dispersibility, good transparency, good luster, good ink absorbency and high dryness.
Description
Technical field
The present invention relates to a kind of preparation method of lime carbonate, relate in particular to a kind of preparation method of Nano calcium carbonate dedicated to printing ink.
Background technology
The fast development of press has driven the development of printing ink calcium carbonate for special use.Show according to printing ink branch of Chinese daily-use chemical industry association integrated information statistical information, national printing ink ultimate production was 250,000 tons in 2002, accounted for 6% of world's printing ink output, compared with last one year that to increase by on a year-on-year basis be 7.32%, sales revenue is 4,600,000,000 yuan, and increasing by on a year-on-year basis is 6.98%.The printing ink ultimate production continues to remain on the 4th in the world, is only second to U.S.'s (1,160,000 tons), Japan's (500,000 tons) and Germany's (450,000 tons).Offset printing ink share maximum wherein accounts for the 40-45% of the total market size.It is predicted that Chinese market will be with annual 9% speed increment to the demand of printing ink, printing-ink output will reach 37.9 ten thousand tons in 2009.China's printing ink industry grows continuously and fast, and output and kind constantly increase, and quality is constantly improved, and class improves constantly, and except that satisfying substantially the domestic needs, product also exports to more than 50 countries and regions such as Eastern Europe, the U.S., Hong Kong, Macao, Taiwan, South East Asia.
Nano-calcium carbonate is used for ink product and has embodied excellent dispersiveness and the transparency and fabulous gloss, and excellent ink absorption and high drying property.Nano-calcium carbonate is made the printing ink filler in resin type printing ink, have good stability, and the glossiness height does not influence the drying property of printing-ink, advantage such as adaptability is strong.
Nano calcium carbonate dedicated to printing ink divides transparent and translucent two big classes, and crystal morphology is cubes or sphere.The particle diameter of transparent ink calcium is at 20-30nm, and the particle diameter of translucent printing ink calcium is about 60nm.Transparent ink calcium becomes the research focus in this field because of its excellent performance, so a kind of preparation method of nanometer transparent mimeograph calcium is provided, and is significant to the quality that improves printing ink.
Carbonization at low temperature (below 20 ℃) is adopted in the preparation of printing ink calcium carbonate for special use at present more, saponification rosin coated caco3, and the lime carbonate particle diameter is little and produce and reunite, and influences dispersiveness, the transparency of product.
Summary of the invention
At the deficiency that prior art exists, the object of the present invention is to provide a kind of preparation method of printing ink dedicated transparent nano-calcium carbonate.
Goal of the invention of the present invention is achieved by the following technical solution:
A kind of preparation method of Nano calcium carbonate dedicated to printing ink, this method in turn includes the following steps:
(1), the natural whiting high-temperature calcination becomes CaO, add cold water then and digest, Ca (OH)
2Slurry;
(2), with Ca (OH)
2Slurry drops in the reactor, adds the crystal formation control agent and stir when 0-15min is carried out in carburizing reagent, and the add-on of crystal formation control agent is the 0.5-2% of weight of calcium carbonate, feeds to contain CO
2Kiln gas carry out carbonization to the pH value of calcium carbonate slurry and reach 7, add the dispersion agent that weight is weight of calcium carbonate 0.1-1% then, it is stand-by to obtain homodisperse nano-calcium carbonate slurry; Wherein carbonization starting temperature is controlled at 15-40 ℃;
(3), adding coating after reaction finishes coats: coating is configured to the aqueous solution, is warmed up to 90-98 ℃, get covering liquid lime carbonate is coated under 60-80 ℃; Described coating is resinous acid and derivative thereof, and the amount of coating is the 1.5-10% of nano-calcium carbonate weight, and the coating time is 20-60 minute;
(4), the lime carbonate after coating is carried out press filtration, drying, drying temperature is 100-120 ℃, nanometer transparent printing ink lime carbonate of the present invention.
In described (1) step the stack gas of calcination of calcium carbonate after purifying as the CO of step (2) carbonization
2Source of the gas, kiln gas CO
2Volume content is 15-25%.
The calcium hydroxide slurry concentration of wherein said step (1) is that 90-120g/L is (with CaCO
3Meter).
Crystal formation control agent described in the step (2) is one or more the mixture in Trisodium Citrate, sucrose, trisodium phosphate, the sodium ethylene diamine tetracetate.
Coating in the described step (3) is rosin, rosined soap, rosin modified phenolic resin, staybelite etc.
According to above method synthetic transparent nanometer calcium carbonate particle diameter at 20-40nm, cubes or sphere, size distribution 1.5-1.6, specific surface is greater than 32m
2/ g, oil-absorption(number) 35-45g/100gCaCO
3, do not have and reunite.The glossiness that records product by standard method is good, transparent, and degree of mobilization is good, is applicable to high-grade offset transparent printing ink filler.
The present invention is according to the crystallization principle of lime carbonate, control the nucleation and the growth velocity of calcium carbonate crystal by control of process condition, in carbonization process, add a certain amount of crystal formation control agent and dispersion agent, with particle diameter and the pattern that need to obtain, and do not have reunion, go out high-quality nanometer transparent mimeograph calcium by coating process for producing.The nano-calcium carbonate that the present invention makes has excellent dispersiveness and the transparency and fabulous gloss, and advantages such as excellent ink absorption and high drying property.
Embodiment
The invention will be further described below by specific examples:
Embodiment 1
Carbonization: adding 1.5 cubic metres of concentration in 2 cubic metres reactor is that 90g/L is (with CaCO
3Meter) calcium hydroxide slurry, 20 ℃ of carbonization starting temperatures add 0.2kg sucrose and 0.3kg Trisodium Citrate before the carbonization, feed to contain CO
2The kiln gas of amount 17-22% (volumetric concentration) carries out carbonization to the pH value of calcium carbonate slurry and reaches 7, adds 0.4kg sodium polyacrylate and 0.2kg zinc chloride then, and it is stand-by to obtain homodisperse nano-calcium carbonate slurry.
Coat: 2.5kg staybelite and 2.5kg dimerization colophonium are dissolved in 95 ℃ the hot water and make covering liquid, then coating is joined in 60 ℃ the nano-calcium carbonate slurry, constant temperature coats 40min, continuous filter press, drying, the nanometer transparent mimeograph calcium.
Finished product: median size is 20nm, and size distribution GSD 1.51, specific surface 45m
2/ g, oil-absorption(number) 47g/100gCaCO
3, do not have and reunite.The glossiness that records product by standard method is good, transparent, and degree of mobilization is good, is applicable to high-grade offset transparent printing ink filler.
Embodiment 2
Carbonization: adding 1.5 cubic metres of concentration in 2 cubic metres reactor is that 120g/L is (with CaCO
3Meter) calcium hydroxide slurry, 15 ℃ of carbonization starting temperatures, feeding contains CO
2The kiln gas of amount 17-22% (volumetric concentration) carries out carbonization, add 0.1kg sodium pyrophosphate and 0.2kg sodium ethylene diamine tetracetate behind the 10min, carbonization to the pH value of calcium carbonate slurry reaches 7, add 0.5kg sodium lauryl sulphate and 0.3kg sal epsom then, it is stand-by to obtain homodisperse nano-calcium carbonate slurry.
Coat: 2kg rosin and 3kg rosin modified phenolic resin are dissolved in 95 ℃ the hot water and make covering liquid, then coating is joined in 60 ℃ the nano-calcium carbonate slurry, constant temperature coats 30min, continuous filter press, drying, the nanometer transparent mimeograph calcium.
Finished product: median size is 30nm, and size distribution GSD 1.55, specific surface 39m
2/ g, oil-absorption(number) 40g/100gCaCO
3, do not have and reunite.The glossiness that records product by standard method is good, transparent, and degree of mobilization is good, is applicable to high-grade offset transparent printing ink filler.
Embodiment 3
Carbonization: adding 1.5 cubic metres of concentration in 2 cubic metres reactor is that 105g/L is (with CaCO
3Meter) calcium hydroxide slurry, 30 ℃ of carbonization starting temperatures add 0.5kg sucrose before the carbonization, feed to contain CO
2The kiln gas of amount 17-22% (volumetric concentration) carries out carbonization, reach at 85% o'clock to carbonation rate and add the 0.3kg Sodium hexametaphosphate 99, continuation carbonization to the pH value of calcium carbonate slurry reaches 7, adds the 0.2kg sodium polyacrylate then, and it is stand-by to obtain homodisperse nano-calcium carbonate slurry.
Coat: the 5kg rosined soap is dissolved in 95 ℃ the hot water and makes covering liquid, then coating is joined in 60 ℃ the nano-calcium carbonate slurry, constant temperature coats 20min, continuous filter press, drying, the nanometer transparent mimeograph calcium.
Finished product: median size is 40nm, and size distribution GSD 1.58, specific surface 32m
2/ g, oil-absorption(number) 36g/100gCaCO
3, do not have and reunite.The glossiness that records product by standard method is good, transparent, and degree of mobilization is good, is applicable to high-grade offset transparent printing ink filler.
Claims (7)
1, a kind of preparation method of Nano calcium carbonate dedicated to printing ink, this method in turn includes the following steps:
(1), the natural whiting high-temperature calcination becomes CaO, add cold water then and digest, Ca (OH)
2Slurry;
(2), with Ca (OH)
2Slurry drops in the reactor, adds the crystal formation control agent and stir when 0-15min is carried out in carburizing reagent, and the add-on of crystal formation control agent is the 0.5-2% of weight of calcium carbonate, feeds to contain CO
2Kiln gas carry out carbonization to the pH value of calcium carbonate slurry and reach 7, add the dispersion agent that weight is weight of calcium carbonate 0.1-1% then, it is stand-by to obtain homodisperse nano-calcium carbonate slurry; Wherein carbonization starting temperature is controlled at 15-40 ℃;
(3), adding coating after reaction finishes coats: coating is configured to the aqueous solution, is warmed up to 90-98 ℃, get covering liquid lime carbonate is coated; Described coating is resinous acid and derivative thereof, and the amount of coating is the 1.5-10% of nano-calcium carbonate weight;
(4), the lime carbonate after coating is carried out press filtration, drying, nanometer transparent printing ink lime carbonate.
2, the preparation method of a kind of high thixotropic nano calcium carbonate according to claim 1 is characterized in that: in described (1) step the stack gas of calcination of calcium carbonate after purifying as the CO of step (2) carbonization
2Source of the gas, kiln gas CO
2Volume content is 15-25%.
3, the preparation method of a kind of high thixotropic nano calcium carbonate according to claim 1 is characterized in that: the temperature of plate in the described step (3) is 60-80 ℃, and the coating time is 20-60 minute.
4, the preparation method of a kind of high thixotropic nano calcium carbonate according to claim 1 is characterized in that: drying temperature is 100-120 ℃ in the described step (4).
5, the preparation method of a kind of Nano calcium carbonate dedicated to printing ink according to claim 1 is characterized in that: the calcium hydroxide slurry concentration of wherein said step (1) is 90-120g/L, with CaCO
3Meter.
6, the preparation method of a kind of Nano calcium carbonate dedicated to printing ink according to claim 1 is characterized in that: the crystal formation control agent described in the step (2) is one or more the mixture in Trisodium Citrate, sucrose, the trisodium phosphate.
7, the preparation method of a kind of Nano calcium carbonate dedicated to printing ink according to claim 1 is characterized in that: the coating in the described step (3) is one or more the mixture in rosin, rosined soap, rosin modified phenolic resin and the staybelite.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510112374 CN1916084A (en) | 2005-12-29 | 2005-12-29 | Method for preparing Nano calcium carbonate dedicated to printing ink |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510112374 CN1916084A (en) | 2005-12-29 | 2005-12-29 | Method for preparing Nano calcium carbonate dedicated to printing ink |
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| CN1916084A true CN1916084A (en) | 2007-02-21 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531391B (en) * | 2009-04-16 | 2011-05-18 | 芜湖卓越纳米新材料有限公司 | Method for industrially preparing nanometer calcium carbonate for solvent type ink addition agent |
| CN103756366A (en) * | 2014-01-09 | 2014-04-30 | 宣城新威华化工科技有限公司 | Preparation method of nano calcium carbonate capable of improving bonding strength of oxime-removing silicone sealant |
| CN105802280A (en) * | 2016-05-20 | 2016-07-27 | 山西新泰恒信纳米材料有限公司 | Preparation method for nano calcium carbonate (CaCO3) for lubricating grease |
| CN107827138A (en) * | 2017-12-08 | 2018-03-23 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of superfine active calcium carbonate |
| CN107963649A (en) * | 2017-12-08 | 2018-04-27 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of super-fine active calcium carbide |
| CN109111762A (en) * | 2018-10-09 | 2019-01-01 | 河南骏化发展股份有限公司 | A kind of preparation method of ink modified nano calcium carbonate |
| CN111393881A (en) * | 2020-05-06 | 2020-07-10 | 国鼎(苏州)材料科技有限公司 | All-inorganic interior and exterior wall coating and preparation method thereof |
| CN112390277A (en) * | 2020-12-07 | 2021-02-23 | 江西华明纳米碳酸钙有限公司 | Preparation method of special nano calcium carbonate for printing ink |
| CN113061353A (en) * | 2021-03-26 | 2021-07-02 | 上海南卓新材料科技有限公司 | Preparation method of filling calcium carbonate for offset printing rotary press ink and product thereof |
| CN113174161A (en) * | 2021-06-16 | 2021-07-27 | 丰城三友制笔科技有限公司 | Printing ink for improving yield value and preparation method thereof |
| CN113353962A (en) * | 2021-06-10 | 2021-09-07 | 襄阳兴发化工有限公司 | Method for preparing active nano calcium carbonate at normal temperature and high concentration |
| CN115367779A (en) * | 2022-08-18 | 2022-11-22 | 襄阳兴发化工有限公司 | Preparation method of nano calcium carbonate with defoaming function for printing ink |
| CN115448347A (en) * | 2022-08-18 | 2022-12-09 | 襄阳兴发化工有限公司 | Preparation method of nano calcium carbonate for ink |
-
2005
- 2005-12-29 CN CN 200510112374 patent/CN1916084A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531391B (en) * | 2009-04-16 | 2011-05-18 | 芜湖卓越纳米新材料有限公司 | Method for industrially preparing nanometer calcium carbonate for solvent type ink addition agent |
| CN103756366A (en) * | 2014-01-09 | 2014-04-30 | 宣城新威华化工科技有限公司 | Preparation method of nano calcium carbonate capable of improving bonding strength of oxime-removing silicone sealant |
| CN103756366B (en) * | 2014-01-09 | 2016-06-29 | 宣城新威华化工科技有限公司 | A kind of preparation method of the nano-calcium carbonate improving de-oxime type silicone sealant adhesive strength |
| CN105802280A (en) * | 2016-05-20 | 2016-07-27 | 山西新泰恒信纳米材料有限公司 | Preparation method for nano calcium carbonate (CaCO3) for lubricating grease |
| CN107827138A (en) * | 2017-12-08 | 2018-03-23 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of superfine active calcium carbonate |
| CN107963649A (en) * | 2017-12-08 | 2018-04-27 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of super-fine active calcium carbide |
| CN109111762A (en) * | 2018-10-09 | 2019-01-01 | 河南骏化发展股份有限公司 | A kind of preparation method of ink modified nano calcium carbonate |
| CN111393881A (en) * | 2020-05-06 | 2020-07-10 | 国鼎(苏州)材料科技有限公司 | All-inorganic interior and exterior wall coating and preparation method thereof |
| CN112390277A (en) * | 2020-12-07 | 2021-02-23 | 江西华明纳米碳酸钙有限公司 | Preparation method of special nano calcium carbonate for printing ink |
| CN113061353A (en) * | 2021-03-26 | 2021-07-02 | 上海南卓新材料科技有限公司 | Preparation method of filling calcium carbonate for offset printing rotary press ink and product thereof |
| CN113353962A (en) * | 2021-06-10 | 2021-09-07 | 襄阳兴发化工有限公司 | Method for preparing active nano calcium carbonate at normal temperature and high concentration |
| CN113174161A (en) * | 2021-06-16 | 2021-07-27 | 丰城三友制笔科技有限公司 | Printing ink for improving yield value and preparation method thereof |
| CN115367779A (en) * | 2022-08-18 | 2022-11-22 | 襄阳兴发化工有限公司 | Preparation method of nano calcium carbonate with defoaming function for printing ink |
| CN115448347A (en) * | 2022-08-18 | 2022-12-09 | 襄阳兴发化工有限公司 | Preparation method of nano calcium carbonate for ink |
| CN115367779B (en) * | 2022-08-18 | 2023-11-24 | 襄阳兴发化工有限公司 | Preparation method of nano calcium carbonate with defoaming function for printing ink |
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