CN103318938A - Method for preparing calcium carbonate special for printing ink - Google Patents

Method for preparing calcium carbonate special for printing ink Download PDF

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Publication number
CN103318938A
CN103318938A CN2013102531674A CN201310253167A CN103318938A CN 103318938 A CN103318938 A CN 103318938A CN 2013102531674 A CN2013102531674 A CN 2013102531674A CN 201310253167 A CN201310253167 A CN 201310253167A CN 103318938 A CN103318938 A CN 103318938A
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calcium carbonate
aqueous solution
printing ink
surface treatment
gained
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CN2013102531674A
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郁平
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SHANGHAI TIANTAN AUXILIARIES CO Ltd
Shanghai Institute of Technology
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SHANGHAI TIANTAN AUXILIARIES CO Ltd
Shanghai Institute of Technology
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Priority to CN2013102531674A priority Critical patent/CN103318938A/en
Publication of CN103318938A publication Critical patent/CN103318938A/en
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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a method for preparing calcium carbonate special for printing ink. The method comprises the following steps: preparing an aqueous solution containing a Ca<2+> ion donor and an aqueous solution containing a CO3<2-> ion donor, controlling the concentration of the Ca<2+> ion to be 0.2-6mol/L and controlling the concentration of the CO3<2-> ion to be 0.2-2mol/L; mixing the aqueous solution containing the Ca<2+> donor and the aqueous solution containing the CO3<2-> ion donor according to the equivalent weight, strongly stirring, reacting for 1-30 minutes, filtering, and performing surface treatment on the obtained filter cake, drying and grinding to obtain calcium carbonate special for printing ink which is uniform in particles, has the particle size of 0.8-2.5 mu m and is well dispersed. Furthermore, because the mother solution obtained by filtering the calcium carbonate can be recycled in the preparation process, the mother solution is used for dissolving a raw material containing the Ca<2+> ion donor and a raw material containing the CO3<2-> ion donor; and therefore, the method is a cleaner production method which has zero discharge and is environment-friendly.

Description

A kind of preparation method of printing ink calcium carbonate for special use
Technical field
The present invention relates to a kind of preparation method of calcium carbonate, particularly a kind of preparation method of calcium carbonate of printing ink special use.
Background technology
Calcium carbonate is widely used in the industries such as plastics, papermaking, coating, printing ink, daily use chemicals.For the calcium carbonate product that is applied to prepare different sorts printing ink, the calcium carbonate granule pattern of requirement has difference, and is also different to the surface treatment requirement of calcium carbonate.As for marking ink, use the pearl filler of spheroidal particle and cube particle, be conducive to clear patterns, seal China ink evenly; For being coated with printing ink, using platy shaped particle can improve coating efficiency and reduce and be coated with the printing ink consumption; For watering down China ink, not only need calcium carbonate granule tiny, and require uniform particles, transparency high.
Calcium carbonate production technique majority is to adopt CO at present 2Pass into Ca (OH) 2The CO of suspension 2Carbonization method, this process is loaded down with trivial details, energy expenditure is large, especially can not adapt to Urban industrial zone for requirement energy-saving and cost-reducing, protection of the environment.Produce the controlled calcium carbonate of particle by liquid-liquid reactions and compare CO 2Carborization is produced calcium carbonate, has more competitive power at aspects such as simple flow, energy efficient, but relevant preparation report seldom.
Chinese invention patent (patent No. ZL 200310122980.4) " a kind of printing ink with the manufacture method of nanometer level calcium carbonate particle " discloses a kind of printing ink with the manufacture method of nanometer level calcium carbonate particle.Add nucleus promotor at the reaction initial period, reach 80% at carbonation rate and add dispersion agent when above, obtain the cube nanometer grade calcium carbonate, but its reaction system is the liming carborization, large energy is wasted in the preparation of milk of lime, therefore and because its solubleness is little can only obtain inhomogeneous suspension system, in the process that generates calcium carbonate, can make calcium carbonate in the calcium hydroxide particle surface coverage, affect the further carbonization of calcium hydroxide, be difficult to simultaneously control the calcium carbonate granule in the same size.
Chinese invention patent (patent No. ZL 01126404.7) " preparation method of transparent nanometer calcium carbonate for high-grade lithographic ink " is by control Ca (OH) 2The temperature of suspension, control CO 2Gas flow is controlled the nucleation rate of calcium carbonate nucleus, and adds the growth velocity that crystal control agent is controlled each crystal face, thereby it is controlled to reach pattern; Continue to add dispersion agent, surface treatment agent adjusting particle surface electric charge and carry out particle surface coating processing, obtained the high-grade lithographic ink filler of particle diameter at 15-40nm.But the particle size distribution of its acquisition is uneven, is difficult to embody stable result of use in the printing ink use procedure.
Summary of the invention
The objective of the invention is in order to solve among the used calcium carbonate preparation method of above-mentioned printing ink, the particle size distribution of final gained is uneven, in the printing ink use procedure, be difficult to embody the technical problems such as stable result of use and provide a kind of uniform particles, particle diameter at 80nm-5 μ m, the preparation method of the calcium carbonate of finely disseminated printing ink special use.
Technical scheme of the present invention
A kind of preparation method of calcium carbonate of printing ink special use specifically comprises the steps:
(1), preparation contains Ca respectively 2+The aqueous solution of ion donor and contain CO 3 2-The aqueous solution of ion donor makes wherein Ca 2+Ionic concn is 0.2-6mol/L, CO 3 2-Ionic concn is 0.2-2mol/L;
The described Ca that contains 2+The donor of ion is calcium chloride water;
The described CO that contains 3 2-The donor of ion is yellow soda ash or wet chemical;
(2), with the Ca that contains of gained in the step (1) 2+The aqueous solution of ion donor and contain CO 3 2-The aqueous solution of ion donor carries out equivalent head-on collision mixing or topples over mixing, and then controlling mixing speed is 300-600rpm, and temperature is 0-80 ℃, reacts 1-30min and obtains calcium carbonate suspension;
It is 0-80 ℃ the Ca that contains that described head-on collision is mixed into temperature 2+The aqueous solution of ion donor and contain CO 3 2-The aqueous solution of ion donor is take flow velocity as 1-12m/s, and angle is that 60-180 ° of head-on collision mixes;
Describedly topple over that to be mixed into temperature be that 0-80 ℃, flow are the Ca that contains of 0.1-2L/s 2+The aqueous solution of ion donor and contain CO 3 2-The aqueous solution of ion donor is toppled over and is mixed;
(3), the calcium carbonate suspension of filtration step (2) gained, the filter cake of gained after deionized water washing in pneumatic conveying dryer, carry out drying passing under 80-150 ℃ the warm air condition, dried calcium carbonate pressed powder control temperature be 70-90 ℃ with after surface treatment agent mixes, the 5-30min that mills in grinding alms bowl is the particle of 80nm-5 μ m to particle diameter, namely gets the calcium carbonate of printing ink special use;
Or with calcium carbonate suspension after filtration, the filter cake of gained control temperature after the deionized water washing is 20-90 ℃, after the adding surface treatment agent mixes, and the 5-30min that in grinding alms bowl, mills, namely getting particle diameter is the calcium carbonate of the printing ink special use of 0.8-2.5 μ m;
Used surface treatment agent is rosin, palmitinic acid or stand linseed oil, and the usage quantity of surface treatment agent is the 1-5% of theoretical gained weight of calcium carbonate;
The filtrate of gained was that the muriate Recycling Mother Solution is used for dissolving raw materials of Ca Cl after the calcium carbonate suspension of gained filtered 2,Yellow soda ash or salt of wormwood after the recycle, are finally produced the muriate crystal in crystallizer.
Beneficial effect of the present invention
The preparation method of the calcium carbonate of a kind of printing ink special use of the present invention is clashed into two strands of liquid materials or is toppled over hybrid reaction, and greatly enhancement of heat transfer, mass transfer process, are saved power at simplification device.Select this reactive mode to be specially adapted to the such mass transfer process of synthetic calcium carbonate and be the moment chemical reaction of control step.The principle of knock-on reaction is that two bursts of high-velocity liquid jet are clashed into certain angle (60～180 °), and material is fully mixed.The principle of toppling over reaction is that two strands of liquid materials are dropped into reactor fast with the form while of equivalent, cooperate simultaneously violent stirring, make the reaction mass in the reactor have the essentially identical reaction times, make calcium carbonate granule size uniformity, its grain diameter is 0.8-2.5 μ m.
Further, the preparation method of the calcium carbonate of a kind of printing ink special use of the present invention is because take rosin or palmitinic acid or stand linseed oil table as surface treatment agent, the calcium carbonate of the final printing ink special use that obtains can be directly used in the preparation of printing ink.(patent No. ZL 200310122980.4, patent No. ZL 01126404.7) compares with prior art, production process of the present invention is simple, and environmentally safe is used more flexible, even can according to the specific requirement of Printing ink producing manufacturer, select suitable surface treatment process.
Further, the preparation method of a kind of printing ink calcium carbonate for special use of the present invention can be that the muriate Recycling Mother Solution is used with filtrate in the preparation process, is used for dissolving raw materials of Ca Cl 2And soluble carbonate salt, so the present invention is the clean preparation method of a kind of zero release, environmentally safe.
Embodiment
Below by specific embodiment the present invention is further set forth, but do not limit the present invention.
Used various raw materials or the specification of reagent and information such as the following table of manufacturer in the various embodiments of the present invention:
Clash into the model of the used various device of reinforced method and information such as the following table of manufacturer in the various embodiments of the present invention:
Manual pressure percussion flow syringe: injector for medical purpose, 200mL, medicine limited-liability company in Shanghai provides;
Agitator, model: RW20.n power: 70W, IKA company limited in Guangzhou produces;
Vacuum pump, model: SHZ-IIIB operating voltage: 220V power: 180W pumping speed (single tube/two-tube): 10/20L/min, Linhai city Seiko vacuum apparatus factory produces;
Pneumatic conveying dryer, model: SK-101, power: 2500W, Shanghai instrument equipment company limited of holy section produces.
Topple over the model of the used various device of reinforced method and information such as the following table of manufacturer in the various embodiments of the present invention:
Agitator, model: RW20.n power: 70W, IKA company limited in Guangzhou produces;
Vacuum pump, model: SHZ-IIIB operating voltage: 220V power: 180W pumping speed (single tube/two-tube): 10/20L/min, Linhai city Seiko vacuum apparatus factory produces.
Pneumatic conveying dryer, model: SK-101, power: 2500W, Shanghai instrument equipment company limited of holy section produces.
Embodiment 1
A kind of preparation method of calcium carbonate of printing ink special use, concrete steps are as follows:
(1), takes by weighing 111gCaCl 2With 106g Na 2CO 3Be made into respectively 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The aqueous solution;
Ca wherein 2+Ionic concn is 2mol/L, CO 3 2-Ionic concn is 2mol/L;
(2), with injector for medical purpose with CaCl 2The aqueous solution and Na 2CO 3The aqueous solution clashes into 90 ° of angles, and the inbound traffics that add of two groups of raw materials are 0.6L/min, and the liquid mixture behind the bump reacts in stirring tank, and stirring velocity is that 400rpm, 20 ℃ of temperature, time are 15min, obtains calcium carbonate suspension after the reaction;
(3), the calcium carbonate suspension of filtration step (2) gained, the filter cake of gained washs through deionized water, be controlled at 20-90 ℃, adding the 150g surface treatment agent is after the 3# stand linseed oil mixes, 15min mills in grinding alms bowl, namely get the 250g particle diameter at 0.8-1.2 μ m, the calcium carbonate CaCO of good dispersion, evengranular printing ink special use 3
Embodiment 2
A kind of preparation method of calcium carbonate of printing ink special use, concrete steps are as follows:
(1), takes by weighing 111gCaCl 2With 106g Na 2CO 3Be made into respectively 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The aqueous solution;
Ca wherein 2+Ionic concn is 2mol/L, CO 3 2-Ionic concn is 2mol/L;
(2), with injector for medical purpose with 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The aqueous solution clashes into 90 ° of angles, 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The inbound traffics that add of the aqueous solution are 0.6L/min, resulting 500ml CaCl behind the bump 2The aqueous solution and 500ml Na 2CO 3Aqueous mixture reacts in stirring tank, and reaction process control stirring velocity is that 400rpm, temperature are that 20 ℃, time are 15min, obtains calcium carbonate suspension after the reaction;
(3), the calcium carbonate suspension of filtration step (2) gained, the filter cake of gained is positioned over temperature and is in 150 ℃ the instrument air dryer and carry out drying after the deionized water washing;
The calcium carbonate pressed powder of gained is after powdery rosin mixes with the 5g surface treatment agent down at 80-90 ℃ after the above-mentioned drying, and the 15min that mills in grinding alms bowl namely gets the 105g particle diameter at 1.5-2.5 μ m, good dispersion, the calcium carbonate CaCO of printing ink special use of uniform size 3
Embodiment 3
A kind of preparation method of calcium carbonate of printing ink special use, concrete steps are as follows:
(1), takes by weighing 111gCaCl 2With 106g Na 2CO 3Be made into respectively 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The aqueous solution;
Ca wherein 2+Ionic concn is 2mol/L, CO 3 2-Ionic concn is 2mol/L;
(2), with injector for medical purpose with 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The aqueous solution clashes into 90 ° of angles, 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The inbound traffics that add of the aqueous solution are 0.6L/min, resulting 500ml CaCl behind the bump 2The aqueous solution and 500ml Na 2CO 3Aqueous mixture reacts in stirring tank, and reaction process control stirring velocity is that 400rpm, 20 ℃ of temperature, time are 15min, obtains calcium carbonate suspension after the reaction;
(3), the calcium carbonate suspension of filtration step (2) gained, the filter cake of gained is positioned over temperature and is in 120 ℃ the instrument air dryer and carry out drying after the deionized water washing;
The calcium carbonate pressed powder of gained is after the powdery palmitinic acid mixes with the 4g surface treatment agent down at 70-80 ℃ after the above-mentioned drying, 15min mills in grinding alms bowl, namely get the 104g particle diameter at 1.5-2.5 μ m, good dispersion, the calcium carbonate CaCO of printing ink special use of uniform size 3
Embodiment 4
A kind of preparation method of calcium carbonate of printing ink special use, concrete steps are as follows:
(1), takes by weighing 111gCaCl 2With 106gNa 2CO 3Be made into respectively 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The aqueous solution;
Ca wherein 2+Ionic concn is 2mol/L, CO 3 2-Ionic concn is 2mol/L;
(2), make 500ml CaCl with toppling over reinforced method 2The aqueous solution and 500ml Na 2CO 3Then aqueous solution, feed time are controlled rotating speed and are 400rpm and stir and make CaCl within 2s 2The aqueous solution and Na 2CO 3Aqueous solution and reaction, 20 ℃ of reaction process control temperature, the time is 15min, obtains calcium carbonate suspension after having reacted;
(3), the calcium carbonate suspension of filtration step (2) gained, the filter cake of gained is after the deionized water washing, be controlled at 20 ℃, adding the 150g surface treatment agent is after the 3# stand linseed oil mixes, 15min mills in grinding alms bowl, namely get the 250g particle diameter at 1.0-1.5 μ m, the calcium carbonate of good dispersion, evengranular printing ink special use.
Embodiment 5
A kind of preparation method of calcium carbonate of printing ink special use, concrete steps are as follows:
(1), takes by weighing 111gCaCl 2With 106gNa 2CO 3Be made into respectively 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The aqueous solution;
Ca wherein 2+Ionic concn is 2mol/L, CO 3 2-Ionic concn is 2mol/L;
(2), make 500ml CaCl with toppling over reinforced method 2The aqueous solution and 500ml Na 2CO 3Aqueous solution, feed time is finished within 2s, and then controlling stirring velocity is that 400rpm stirs, and makes CaCl 2The aqueous solution and Na 2CO 3Aqueous solution and reaction, 20 ℃ of reaction process control temperature, the time is 15min, obtains calcium carbonate suspension after having reacted;
(3), the calcium carbonate suspension of filtration step (2) gained, the filter cake of gained is positioned over temperature and is in 150 ℃ the instrument air dryer and carry out drying after the deionized water washing;
The calcium carbonate pressed powder of gained is after powdery rosin mixes with the 5g surface treatment agent down at 80-90 ℃ after the above-mentioned drying, and the 15min that mills in grinding alms bowl namely gets the 105g particle diameter at 1.0-1.5 μ m, good dispersion, the calcium carbonate of printing ink special use of uniform size.
Embodiment 6
A kind of preparation method of calcium carbonate of printing ink special use, concrete steps are as follows:
(1), takes by weighing 111gCaCl 2With 106gNa 2CO 3Be made into respectively 500ml CaCl 2The aqueous solution and 500ml Na 2CO 3The aqueous solution;
Ca wherein 2+Ionic concn is 2mol/L, CO 3 2-Ionic concn is 2mol/L;
(2), make 500ml CaCl with toppling over reinforced method 2The aqueous solution and 500ml Na 2CO 3The aqueous solution mixes, and total dumping time is within 2s, and then controlling stirring velocity is that 400rpm stirs, and makes CaCl 2The aqueous solution and Na 2CO 3Aqueous solution and reaction, 20 ℃ of reaction process control temperature, the time is 15min, obtains calcium carbonate suspension after having reacted;
(3), the calcium carbonate suspension of filtration step (2) gained, the filter cake of gained is positioned over temperature and is in 80 ℃ the instrument air dryer and carry out drying after the deionized water washing;
The calcium carbonate pressed powder of gained is after the powdery palmitinic acid mixes with the 4g surface treatment agent down at 70-80 ℃ after the above-mentioned drying, and the 15min that mills in grinding alms bowl namely gets the 104g particle diameter at 1-1.5 μ m, good dispersion, the calcium carbonate of printing ink special use of uniform size.
Foregoing only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.

Claims (7)

1. the preparation method of the calcium carbonate of a printing ink special use is characterized in that specifically comprising the steps:
(1), preparation contains Ca respectively 2+The aqueous solution of ion donor and contain CO 3 2-The aqueous solution of ion donor, wherein Ca 2+Ionic concn is 0.2-6mol/L, CO 3 2-Ionic concn is 0.2-2mol/L;
(2), with the Ca that contains of gained in the step (1) 2+The aqueous solution of ion donor and contain CO 3 2-After the aqueous solution of ion donor clashed and mixes or topple over mixing, the control mixing speed was that 300-600rpm, temperature are 0-80 ℃, reacts 1-30min and obtains calcium carbonate suspension;
(3), with the calcium carbonate suspension of step (2) gained after filtration, drying, surface treatment, milling namely obtains the calcium carbonate of printing ink special use;
Or with the calcium carbonate suspension of step (2) gained after filtration, surface treatment, milling obtains the calcium carbonate of printing ink special use.
2. the preparation method of the calcium carbonate of a kind of printing ink special use as claimed in claim 1 is characterized in that the described Ca of containing of step (1) 2+The aqueous solution of the donor of ion is calcium chloride water.
3. the preparation method of a kind of printing ink calcium carbonate for special use as claimed in claim 2 is characterized in that the described CO of containing of step (1) 3 2-The aqueous solution of the donor of ion is yellow soda ash or wet chemical.
4. such as the preparation method of the calcium carbonate of claim 1,2 or 3 described a kind of printing ink special uses, it is characterized in that the described Ca of step (1) 2+Ionic concn is 2mol/L, CO 3 2-Ionic concn is 2mol/L.
5. a kind of preparation method of calcium carbonate of printing ink special use as claimed in claim 4 is characterized in that it is 0-80 ℃ the Ca that contains that the described head-on collision of step (2) is mixed into temperature 2+The aqueous solution of ion donor and contain CO 3 2-The aqueous solution of ion donor is take flow velocity as 1-12m/s, and angle is that 60-180 ° of head-on collision mixes;
Describedly topple over that to be mixed into temperature be that 0-80 ℃, flow are the Ca that contains of 0.1-2L/s 2+The aqueous solution of ion donor and contain CO 3 2-The aqueous solution of ion donor is toppled over and is mixed.
6. a kind of preparation method of calcium carbonate of printing ink special use as claimed in claim 1, it is characterized in that step (3) is described after filtration, drying, surface treatment, mill, namely filter the calcium carbonate suspension of gained, the filter cake of gained after deionized water washing in pneumatic conveying dryer, pass under 80-150 ℃ the warm air condition and carry out drying, dried calcium carbonate pressed powder control temperature be 70-90 ℃ with after surface treatment agent mixes, the 5-30min that mills in the stone roller alms bowl gets final product;
Used surface treatment agent is that particle diameter is colophonium powder, palmitinic acid powder or the stand linseed oil of 0.1-1mm, and the consumption of surface treatment agent is the 1-5% of theoretical gained weight of calcium carbonate.
7. the preparation method of the calcium carbonate of a kind of printing ink special use as claimed in claim 1, the calcium carbonate suspension filtration that it is characterized in that described filtration, surface treatment, mills and be about to gained, the filter cake of gained is controlled temperature at 20-90 ℃ after the deionized water washing, after the adding surface treatment agent mixed, the 5-30min that mills in grinding alms bowl got final product;
Used surface treatment agent is that particle diameter is rosin, palmitinic acid or the stand linseed oil of 0.1-1mm, and the consumption of surface treatment agent is the 1-5% of theoretical gained weight of calcium carbonate.
CN2013102531674A 2013-06-25 2013-06-25 Method for preparing calcium carbonate special for printing ink Pending CN103318938A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1634767A (en) * 2003-12-30 2005-07-06 上海华明高技术（集团）有限公司 Method for producing nano calcium carbonate particles for printing ink
CN1757597A (en) * 2005-10-25 2006-04-12 上海应用技术学院 Method for preparing porous super fine calcium carbonate
CN102365236A (en) * 2009-03-27 2012-02-29 白石工业株式会社 Surface-treated calcium carbonate and paste resin composition containing same
CN102910662A (en) * 2012-10-25 2013-02-06 上海应用技术学院 Preparation method of granularity-controllable CaCO3

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1634767A (en) * 2003-12-30 2005-07-06 上海华明高技术（集团）有限公司 Method for producing nano calcium carbonate particles for printing ink
CN1757597A (en) * 2005-10-25 2006-04-12 上海应用技术学院 Method for preparing porous super fine calcium carbonate
CN102365236A (en) * 2009-03-27 2012-02-29 白石工业株式会社 Surface-treated calcium carbonate and paste resin composition containing same
CN102910662A (en) * 2012-10-25 2013-02-06 上海应用技术学院 Preparation method of granularity-controllable CaCO3

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Application publication date: 20130925