CN1264753C - Preparation method of lamellar crystal light calcium carbonate for paper making coating - Google Patents
Preparation method of lamellar crystal light calcium carbonate for paper making coating Download PDFInfo
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- CN1264753C CN1264753C CN 200410093828 CN200410093828A CN1264753C CN 1264753 C CN1264753 C CN 1264753C CN 200410093828 CN200410093828 CN 200410093828 CN 200410093828 A CN200410093828 A CN 200410093828A CN 1264753 C CN1264753 C CN 1264753C
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Abstract
The present invention belongs to the technical field of inorganic synthesis, and relates to a preparation method of flaky crystal light calcium carbonate for coating paper. The present invention is characterized in that the method comprises the following steps of preparing soluble calcium salts into a solution, preparing soluble carbonate into a solution, adding one solution to the other one solution at certain temperature, preparing superfine calcium carbonate seed crystals through reactions, proportionally adding the superfine calcium carbonate seed crystals and mother liquor to purified lime cream, evenly mixing the mixtures, controlling a temperature range, leading in carbon dioxide with certain flow capacity, carbonizing the mixtures to end point, and filtering and drying slurry to obtain flaky crystal light calcium carbonate for coating paper, and the average grain diameter of the light calcium carbonate is from 0.2 to 0.7 mum. The product mother liquor can be recovered and used for dissolving calcium salts or carbonate.
Description
Technical field:
The invention belongs to inorganic synthesis technical field, the preparation method of a kind of lamellar crystal light calcium carbonate for paper making coating of further saying so.
Background technology:
Lime carbonate is the very large mineral filler of a kind of consumption, is widely used in industries such as papermaking, plastics, rubber, printing ink, medicine.At present, family surplus the national factory 300, yearly capacity reaches 5,300,000 tons, about 4,200,000 tons of actual output.Yet major part is common light calcium carbonate and low-grade water-ground limestone, and they can only be used for plastics, rubber and paper industry and make general filler, and added value of product is not high.In recent years, along with the rise of nano material, the research of nano-calcium carbonate is also very active, and has obtained good achievement.And as having the papermaking calcium carbonate for special use of huge market potential, be better kind with the form of flake crystal lime carbonate of submicron order particle diameter, but because the preparation relative difficult, so the rare breakthrough of investigator.
In the past, in the mineral filler and coating pigment of paper grade (stock), using more is kaolin, it has obtained historical achievement, but along with the transformation of the acid applying glue of paper industry to neutrality or alkaline bleach liquor sizing, lime carbonate has the stacking factor bigger than kaolin, lower production cost, especially high-quality lime carbonate has more the unrivaled performance of kaolin in White Board, text paper, and it is low in China's kaolin ore grade, and the lime carbonate mineral is excellent, reserves are big, so in paper industry, lime carbonate is replacing kaolin gradually becomes main filling component.In paper grade (stock) lime carbonate, comprise FGCC (Fine Heavy Calcium Carbonate) and PCC (light calcium carbonate), they are used for paper industry and mainly make filler and coating pigment, as coating pigment, FGCC generally adopts the Pd60 level to be used for primary coat, the Pd90 level is used for face and is coated with, its advantage is that rheological is good, and shortcoming is the ingredient requirement height, to silk screen serious wear etc.; PCC is then according to the external light calcium carbonate that shows the form of flake crystal of selecting uniformly certain particle diameter for use of using, can obtain very excellent sheet coating effect, it has not only overcome the shortcoming of FGCC, and has high whiteness, high opaqueness, high smoothness and good absorbency and advantages such as gloss, coating good fluidity.Therefore, the flaky calcium carbonate of the special-purpose certain particle diameter of research and development papermaking is very necessary and urgent.
The preparation method of existing papermaking flaky precipitate lime carbonate generally is divided into emulsion method and carborization.Emulsion method is meant in certain emulsion medium, adds certain calcium salt and certain carbonate, under certain conditions, utilizes emulsion to limit for the crystallization spatial and prepares flaky calcium carbonate, and this method preparation cost is higher, is restricted aspect industrialization; And carborization is meant the light calcium carbonate preparation technology that employing is traditional, in carbonization process, add crystal control agent, dispersion agent waits and prepares flaky calcium carbonate, this method report has and adopts organic seeing thing to make control agent, also have and adopt boride to make control agent, the former is because organic seeing costs an arm and a leg and toxicity should not adopt greatly, and the latter has obtained certain effect according to report.
Summary of the invention:
The present invention is all inequality with existing emulsion method and carborization.The present invention makes the fine crystal seed of the lime carbonate that is scattered in its mother liquor with the calcium salt of solubility and the carbonate of solubility with specific precipitin reaction condition earlier, and then feed carbonic acid gas under given conditions after crystal seed and mother liquor thereof added milk of lime in specific ratio, make paper making and cloth coating form of flake crystal lime carbonate by strict carbonization condition.
Technical characterstic key one of the present invention is will be by strictly controlling the lime carbonate crystal seed that the precipitin reaction condition prepares fine and high dispersing, the 2nd, prepare form of flake crystal calcium carbonate powder by strictly controlling the carburizing reagent condition with granularity requirements.
The present invention is a kind of preparation method of lamellar crystal light calcium carbonate for paper making coating, it is characterized in that technological process comprises: elder generation is with the calcium salt of one or more solubilities, comprising nitrocalcite, calcium chloride, calcium acetate, be made into 5～20% solution, again with one or more soluble carbon hydrochlorates, comprising yellow soda ash, salt of wormwood, volatile salt, sodium bicarbonate, saleratus, bicarbonate of ammonia, be made into 10～30% solution, then in temperature is 10～50 ℃ of scopes, calcium salt soln is slowly joined carbonate solution or carbonate solution is slowly joined calcium salt soln, prepare the fine crystal seed of lime carbonate by reaction; Other is proportioning according to dosage, calcium oxide is digested, makes the milk of lime of 1%-15% concentration; The fine crystal seed of lime carbonate is joined in the milk of lime in 3%～60% ratio together with its mother liquor, and mixing, controlled temperature are under 10～70 ℃ of scopes, and the feeding flow is 5-50L/min.kgCa (OH)
2Carbonic acid gas, carbonization is to terminal; Slip is through the form of flake crystal paper making and cloth coating light calcium carbonate that filters, drying obtains median size 0.2～0.7 μ m.Its product mother liquid reclaims again, in order to dissolving calcium salt or carbonate.
As the preferred technical solution of the present invention, it is characterized in that technological process comprises: elder generation is with the calcium salt of solubility, be made into 10～20% solution, again the soluble carbon hydrochlorate is made into the solution of 20-30%, then in temperature is 30～40 ℃ of scopes, calcium salt soln is slowly joined carbonate solution or carbonate solution is slowly joined calcium salt soln, prepare the fine crystal seed of lime carbonate by reaction; Other is proportioning according to dosage, calcium oxide is digested, makes the milk of lime of 4%-12% concentration; The fine crystal seed of lime carbonate is joined in the milk of lime in 3%～40% ratio together with its mother liquor, and mixing, controlled temperature are under 10～30 ℃ of scopes, and the feeding flow is 30-40L/min.kgCa (OH)
2Carbonic acid gas, carbonization is to terminal.
As the technical scheme of more optimizing, of the present invention being further characterized in that:
Preparing by precipitin reaction in the process of the fine crystal seed of lime carbonate, the calcium salt of solubility with calcium chloride for well, used soluble carbon hydrochlorate with volatile salt or yellow soda ash for well.The order that adds for calcium salt soln join carbonate solution or carbonate solution join calcium salt soln all can, and join in the carbonate solution to well with calcium salt soln.
The calcium salt of solubility is made into 10～15% solution, and used soluble carbon hydrochlorate is made into 20～25% solution.
The precipitation reaction temperature scope is 30-35 ℃.
Calcium oxide is digested, makes the milk of lime of 5%-8% concentration.
The carbonization temperature scope is 25-30 ℃.
Is 3%-8% with the fine crystal seed of lime carbonate together with the ratio that its mother liquor joins in the milk of lime.
During carbonization, the feeding flow is 30-35L/min.kgCa (OH)
2Carbonic acid gas.
Characteristics of the present invention and positively effect: the present invention adopts the method for introducing crystal seed, and carbonization milk of lime prepares the form of flake crystal paper making and cloth coating light calcium carbonate of median size 0.2 ~ 0.7 μ m under certain conditions.Crystal seed preparation manipulation crucial among the present invention is simple.The present invention is except the preparation of crystal seed, and all the other equipment and the common lightweight carbonic acid of production are basic identical, are easy to industrialization.The lamellar crystal light calcium carbonate of median size 0.2 ~ 0.7 μ m by the present invention preparation adapts to the requirement of paper making and cloth coating with lime carbonate.
Embodiment:
Embodiment one:
Take by weighing 11g calcium chloride and be made into 6% aqueous solution, take by weighing 10.4g salt of wormwood again and be made into 10% solution, temperature adjustment to 15 ℃, solution of potassium carbonate is slowly joined calcium chloride solution make 7.5g lime carbonate crystal seed, join the crystal seed for preparing in the milk of lime of 2716mL5% together with its mother liquor, temperature adjustment to 12 ℃, control CO
2Flow be 0.38m
3/ h. carries out carburizing reagent, and carbonization is behind terminal point, and product is through filtration, the dry finished product that gets.Finished product transmission electron microscope observation, its crystalline median size are 0.4 μ m, and crystalline form is a sheet.
Embodiment two:
Take by weighing 120g nitrocalcite and be made into 10% aqueous solution, take by weighing 60g bicarbonate of ammonia again and be made into 15% solution, temperature adjustment to 25 ℃, ca nitrate soln is slowly joined ammonium bicarbonate soln make 50g lime carbonate crystal seed, join the crystal seed for preparing in the milk of lime of 934mL12% together with its mother liquor, temperature adjustment to 30 ℃, control CO
2Flow be 0.13m
3/ h carries out carburizing reagent, and carbonization is behind terminal point, and product is through filtration, the dry finished product that gets.Finished product transmission electron microscope observation, its crystalline median size are 0.6 μ m, and crystalline form is a sheet.
Embodiment three:
Take by weighing the 105.6g calcium acetate and 95.6g calcium chloride respectively is made into 20% aqueous solution, take by weighing the 80g sodium bicarbonate again and the 30g saleratus respectively is made into 30% solution, temperature adjustment to 30 ℃, calcium acetate and calcium chloride mixing solutions are slowly joined in the sodium bicarbonate saleratus mixing solutions, make 125g lime carbonate crystal seed, the crystal seed for preparing is joined in the milk of lime of 875mL8% temperature adjustment to 45 ℃, control CO together with its mother liquor
2Flow be 0.27m
3/ h carries out carburizing reagent, and carbonization is behind terminal point, and product is through filtration, the dry finished product that gets.Finished product transmission electron microscope observation, its crystalline median size are 0.5 μ m, and crystalline form is a sheet.
Claims (9)
1. the preparation method of a lamellar crystal light calcium carbonate for paper making coating, it is characterized in that technological process comprises: elder generation is with the calcium salt of one or more solubilities, comprising nitrocalcite, calcium chloride, calcium acetate, be made into 5～20% solution, again with one or more soluble carbon hydrochlorates, comprising yellow soda ash, salt of wormwood, volatile salt, sodium bicarbonate, saleratus, bicarbonate of ammonia, be made into 10～30% solution, then in 10～50 ℃ of scopes of temperature, calcium salt soln is slowly joined carbonate solution or carbonate solution is slowly joined calcium salt soln, prepare the fine crystal seed of lime carbonate by reaction; Other is proportioning according to dosage, calcium oxide is digested, makes the milk of lime of 1%-15% concentration; The fine crystal seed of lime carbonate is joined in the milk of lime in 3%～60% ratio together with its mother liquor, and mixing, controlled temperature are 10～70 ℃ of scopes, and the feeding flow is 5-50L/min.kgCa (OH)
2Carbonic acid gas, carbonization is to terminal; Slip is through the form of flake crystal paper making and cloth coating light calcium carbonate that filters, drying obtains median size 0.2～0.7 μ m, and its product mother liquid reclaims again, in order to dissolving calcium salt or carbonate.
2. method according to claim 1, it is further characterized in that technological process comprises: elder generation is with the calcium salt of solubility, be made into 10～20% solution, again the soluble carbon hydrochlorate is made into the solution of 20-30%, then in temperature is 30～40 ℃ of scopes, calcium salt soln is slowly joined carbonate solution or carbonate solution is slowly joined calcium salt soln, prepare the fine crystal seed of lime carbonate by reaction; Other is proportioning according to dosage, calcium oxide is digested, makes the milk of lime of 4%-12% concentration; The fine crystal seed of lime carbonate is joined in the milk of lime in 3%～40% ratio together with its mother liquor, and mixing, controlled temperature are 10～30 ℃ of scopes, and the feeding flow is 30-40L/min.kgCa (OH)
2Carbonic acid gas, carbonization is to terminal.
3. method according to claim 2, it is further characterized in that and is preparing by precipitin reaction in the process of the fine crystal seed of lime carbonate, the calcium salt of solubility is a calcium chloride, and used soluble carbon hydrochlorate is volatile salt or yellow soda ash, and the order of adding joins carbonate solution for calcium salt soln.
4. method according to claim 2, the calcium salt that it is further characterized in that solubility is made into 10～15% solution, and used soluble carbon hydrochlorate is made into 20～25% solution.
5. method according to claim 2, it is further characterized in that the precipitation reaction temperature scope is 30-35 ℃.
6. method according to claim 2, it is further characterized in that the milk of lime that calcium oxide is digested, makes 5%-8% concentration.
7. method according to claim 2, it is further characterized in that the carbonization temperature scope is 25-30 ℃.
8. method according to claim 2, it is further characterized in that be 3%-8% with the fine crystal seed of lime carbonate together with the ratio that its mother liquor joins in the milk of lime.
9. method according to claim 2, when it was further characterized in that carbonization, the feeding flow was 30-35L/min.kgCa (OH)
2Carbonic acid gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200410093828 CN1264753C (en) | 2004-12-03 | 2004-12-03 | Preparation method of lamellar crystal light calcium carbonate for paper making coating |
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| CN 200410093828 CN1264753C (en) | 2004-12-03 | 2004-12-03 | Preparation method of lamellar crystal light calcium carbonate for paper making coating |
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| CN1264753C true CN1264753C (en) | 2006-07-19 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935866B (en) * | 2010-09-16 | 2012-01-25 | 河南城建学院 | Method for preparing flaky calcite calcium carbonate crystal |
| CN103950965B (en) * | 2014-04-29 | 2016-07-13 | 东华大学 | A kind of method using kind of crystallization to prepare different size nano-calcium carbonate |
| EP3012223A1 (en) * | 2014-10-24 | 2016-04-27 | Omya International AG | PCC with reduced portlandite content |
| CN105645451A (en) * | 2016-02-25 | 2016-06-08 | 青海盐湖工业股份有限公司 | Method for preparing micropowder-grade light calcium carbonate |
| CN105883880A (en) * | 2016-04-07 | 2016-08-24 | 安徽江东科技粉业有限公司 | Preparation method of sheet superfine calcium carbonate for paper coating |
| CN106830044A (en) * | 2017-04-17 | 2017-06-13 | 华东理工大学 | A kind of preparation method of the narrow fine particle calcium carbonate of particle diameter distribution |
| CN107758718B (en) * | 2017-11-17 | 2020-08-28 | 池州市富华粉体科技有限公司 | Method for preparing superfine calcium carbonate nano powder from calcite |
| CN112678839B (en) * | 2019-10-18 | 2022-07-01 | 中国科学院过程工程研究所 | Preparation method of calcium silicate with controllable particle size, calcium silicate prepared by preparation method and application of calcium silicate |
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