CN112456532B - Preparation method of calcium carbonate - Google Patents
Preparation method of calcium carbonate Download PDFInfo
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- CN112456532B CN112456532B CN202011441604.1A CN202011441604A CN112456532B CN 112456532 B CN112456532 B CN 112456532B CN 202011441604 A CN202011441604 A CN 202011441604A CN 112456532 B CN112456532 B CN 112456532B
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- Prior art keywords
- thick film
- ethanol
- calcium carbonate
- calcium chloride
- amyl alcohol
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 70
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 28
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 27
- 239000001110 calcium chloride Substances 0.000 claims abstract description 27
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 27
- 238000001556 precipitation Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000005507 spraying Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- 235000019441 ethanol Nutrition 0.000 claims abstract description 17
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 16
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 16
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 16
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 16
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 239000006185 dispersion Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 11
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 238000000643 oven drying Methods 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011575 calcium Substances 0.000 abstract description 4
- 229910052791 calcium Inorganic materials 0.000 abstract description 4
- 239000002245 particle Substances 0.000 description 9
- 239000012752 auxiliary agent Substances 0.000 description 8
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 4
- 229940043264 dodecyl sulfate Drugs 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
Classifications
-
- 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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention belongs to the field of logistics labels, and particularly relates to a preparation method of calcium carbonate, which comprises the following steps: adding calcium chloride into absolute ethyl alcohol, and stirring carboxymethyl cellulose and sodium dodecyl sulfate at constant temperature until the calcium chloride and the sodium dodecyl sulfate are completely dissolved to obtain a dispersion suspension; spraying the dispersion suspension on a substrate, drying to obtain a mixed film, and repeating the operation for 10-200 times to obtain a mixed thick film; placing the mixed thick film in a reaction kettle, placing the mixed thick film at the middle end of the reaction kettle, introducing n-amyl alcohol-water layering liquid at room temperature until the mixed thick film is completely settled, and filtering to obtain crystal precipitation; adding ethanol into the filtrate obtained in the step 3, stirring uniformly until precipitation is no longer generated, and filtering to obtain secondary precipitation; the addition amount of the ethanol is 100-130% of the mass of the n-amyl alcohol, and the stirring speed is 1000-2000r/min; and mixing and washing the precipitate, and drying to obtain the calcium carbonate. The invention utilizes the different solubilities of the calcium materials to form rapid conversion, thus realizing the nano precipitation of calcium carbonate.
Description
Technical Field
The invention belongs to the field of logistics labels, and particularly relates to a preparation method of calcium carbonate.
Background
In the production process of logistics labels, calcium carbonate is one of the most commonly used fillers, and the light calcium carbonate prepared by the current calcium carbonate process contains a large amount of auxiliary agents as additives, so that the purity of the calcium carbonate is low, a large amount of impurities are contained, the impurities are difficult to remove, and the process cost is greatly increased. When the material is added to a material label, the particle size and purity of the calcium carbonate influence the bulk density, apparent fineness and water absorption of paper.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of calcium carbonate, which solves the problem of purity reduction caused by excessive auxiliary agents in the prior calcium carbonate process, and realizes nano precipitation of calcium carbonate by utilizing the rapid conversion formed by different solubilities of calcium materials.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a method for preparing calcium carbonate, comprising the following steps:
step 1, adding calcium chloride into absolute ethyl alcohol, and stirring carboxymethyl cellulose and sodium dodecyl sulfate at constant temperature until the carboxymethyl cellulose and the sodium dodecyl sulfate are completely dissolved to obtain a dispersion suspension; the concentration of the calcium chloride in the absolute ethyl alcohol is 100-250g/L, the adding amount of the carboxymethyl cellulose is 30-50% of the mass of the calcium chloride, the adding amount of the dodecyl sulfate is 5-10% of the mass of the calcium chloride, the constant temperature stirring temperature is 50-60 ℃, and the stirring speed is 1000-2000r/min;
step 2, dividingSpraying the suspension onto a substrate, oven drying to obtain a mixed film, repeating the above steps for 10-200 times to obtain a mixed thick film, wherein the spraying amount of the spray is 5-10g/cm 2 Spraying at 50-60deg.C and oven drying at 80-90deg.C;
step 3, placing the mixed thick film in a reaction kettle, placing the mixed thick film at the middle end of the reaction kettle, introducing n-amyl alcohol-water layering liquid at room temperature until the mixed thick film is completely settled, and filtering to obtain crystal precipitation; the room temperature is 10-20 ℃, the volume ratio of n-amyl alcohol to water in the layering liquid of n-amyl alcohol and water is 1:3-6, the mixed thick film is arranged in n-amyl alcohol, sodium carbonate is dissolved in water, and the adding amount of sodium carbonate is 100-120% of the mass of calcium chloride;
step 4, adding ethanol into the filtrate filtered in the step 3 and stirring uniformly until precipitation is no longer generated, and filtering to obtain secondary precipitation; the addition amount of the ethanol is 100-130% of the mass of the n-amyl alcohol, and the stirring speed is 1000-2000r/min;
and 5, mixing and washing the precipitate in the step 3 and the step 4, and drying to obtain calcium carbonate, wherein the washing adopts an ethanol water solution, the volume concentration of ethanol in the ethanol water solution is 70-80%, and the drying temperature is 100-120 ℃.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of purity reduction caused by excessive auxiliary agents in the existing calcium carbonate technology, and realizes nano precipitation of calcium carbonate by utilizing the rapid conversion formed by different solubilities of calcium materials.
2. The invention uses the conversion of the solvent to control the dissolution change of the auxiliary agent, effectively solves the residual problem of the auxiliary agent, and improves the purity of the calcium carbonate.
3. The preparation method provided by the invention does not need high-temperature sintering, does not damage the chemical properties of raw materials, and can recycle the dispersing agent and the solvent.
4. The calcium carbonate prepared by the method has uniform particle size distribution and strong controllability, and shows good adsorptivity and stability in the field of material labels, so that the printing definition is improved, and the quality of the labels is greatly improved.
Detailed Description
The invention is described in detail with reference to examples, but without any limitation to the claims of the invention.
Example 1
A method for preparing calcium carbonate, comprising the following steps:
step 1, adding calcium chloride into 1L of absolute ethyl alcohol, and stirring carboxymethyl cellulose and sodium dodecyl sulfate at constant temperature until the carboxymethyl cellulose and the sodium dodecyl sulfate are completely dissolved to obtain a dispersion suspension; the concentration of the calcium chloride in the absolute ethyl alcohol is 100g/L, the adding amount of the carboxymethyl cellulose is 30% of the mass of the calcium chloride, the adding amount of the dodecyl sulfate is 5% of the mass of the calcium chloride, the constant-temperature stirring temperature is 50 ℃, and the stirring speed is 1000r/min;
step 2, spraying the dispersion suspension on a substrate, drying to obtain a mixed film, repeating the operation for 10 times according to the operation to obtain a mixed thick film, wherein the spraying amount of the spraying is 5g/cm 2 Spraying at 50-60deg.C and oven drying at 80deg.C;
step 3, placing the mixed thick film in a reaction kettle, placing the mixed thick film at the middle end of the reaction kettle, introducing n-amyl alcohol-water layering liquid at room temperature until the mixed thick film is completely settled, and filtering to obtain crystal precipitation; the room temperature is 10 ℃, the volume ratio of n-amyl alcohol to water in the layering liquid of n-amyl alcohol and water is 1:3, the mixed thick film is arranged in n-amyl alcohol, sodium carbonate is dissolved in water, and the adding amount of sodium carbonate is 100% of the mass of calcium chloride;
step 4, adding ethanol into the filtrate filtered in the step 3 and stirring uniformly until precipitation is no longer generated, and filtering to obtain secondary precipitation; the addition amount of the ethanol is 100% of the mass of the n-amyl alcohol, and the stirring speed is 1000r/min;
and 5, mixing and washing the precipitate in the step 3 and the step 4, and drying to obtain calcium carbonate, wherein the washing adopts an ethanol water solution, the volume concentration of ethanol in the ethanol water solution is 70%, and the drying temperature is 100 ℃.
The average particle diameter of the nano calcium carbonate prepared in the embodiment is 700nm, wherein the particle content of 0-900nm is 93%, and the purity reaches 98.3%.
Example 2
A method for preparing calcium carbonate, comprising the following steps:
step 1, adding calcium chloride into 1L of absolute ethyl alcohol, and stirring carboxymethyl cellulose and sodium dodecyl sulfate at constant temperature until the carboxymethyl cellulose and the sodium dodecyl sulfate are completely dissolved to obtain a dispersion suspension; the concentration of the calcium chloride in the absolute ethyl alcohol is 250g/L, the adding amount of the carboxymethyl cellulose is 50% of the mass of the calcium chloride, the adding amount of the dodecyl sulfate is 10% of the mass of the calcium chloride, the constant-temperature stirring temperature is 60 ℃, and the stirring speed is 2000r/min;
step 2, spraying the dispersion suspension on a substrate, drying to obtain a mixed film, repeating the operation for 200 times according to the operation to obtain a mixed thick film, wherein the spraying amount of the spraying is 10g/cm 2 Spraying at 60deg.C and oven drying at 90deg.C;
step 3, placing the mixed thick film in a reaction kettle, placing the mixed thick film at the middle end of the reaction kettle, introducing n-amyl alcohol-water layering liquid at room temperature until the mixed thick film is completely settled, and filtering to obtain crystal precipitation; the room temperature is 20 ℃, the volume ratio of n-amyl alcohol to water in the layering liquid of n-amyl alcohol and water is 1:6, the mixed thick film is arranged in n-amyl alcohol, sodium carbonate is dissolved in water, and the adding amount of sodium carbonate is 120% of the mass of calcium chloride;
step 4, adding ethanol into the filtrate filtered in the step 3 and stirring uniformly until precipitation is no longer generated, and filtering to obtain secondary precipitation; the addition amount of the ethanol is 130% of the mass of the n-amyl alcohol, and the stirring speed is 2000r/min;
and 5, mixing and washing the precipitate in the step 3 and the step 4, and drying to obtain calcium carbonate, wherein the washing adopts an ethanol water solution, the volume concentration of ethanol in the ethanol water solution is 80%, and the drying temperature is 120 ℃.
The average particle diameter of the nano calcium carbonate prepared in the embodiment is 800nm, wherein the particle content of 0-900nm is 91%, and the purity reaches 98.7%.
Example 3
A method for preparing calcium carbonate, comprising the following steps:
step 1, adding calcium chloride into 1L of absolute ethyl alcohol, and stirring carboxymethyl cellulose and sodium dodecyl sulfate at constant temperature until the carboxymethyl cellulose and the sodium dodecyl sulfate are completely dissolved to obtain a dispersion suspension; the concentration of the calcium chloride in the absolute ethyl alcohol is 150g/L, the adding amount of the carboxymethyl cellulose is 40% of the mass of the calcium chloride, the adding amount of the dodecyl sulfate is 8% of the mass of the calcium chloride, the constant-temperature stirring temperature is 55 ℃, and the stirring speed is 1500r/min;
step 2, spraying the dispersion suspension on a substrate, drying to obtain a mixed film, repeating the operation for 150 times according to the operation to obtain a mixed thick film, wherein the spraying amount of the spraying is 8g/cm 2 The spraying temperature is 55 ℃, and the drying temperature is 85 ℃;
step 3, placing the mixed thick film in a reaction kettle, placing the mixed thick film at the middle end of the reaction kettle, introducing n-amyl alcohol-water layering liquid at room temperature until the mixed thick film is completely settled, and filtering to obtain crystal precipitation; the room temperature is 15 ℃, the volume ratio of n-amyl alcohol to water in the layering liquid of n-amyl alcohol and water is 1:5, the mixed thick film is arranged in n-amyl alcohol, sodium carbonate is dissolved in water, and the adding amount of sodium carbonate is 110% of the mass of calcium chloride;
step 4, adding ethanol into the filtrate filtered in the step 3 and stirring uniformly until precipitation is no longer generated, and filtering to obtain secondary precipitation; the addition amount of the ethanol is 120% of the mass of the n-amyl alcohol, and the stirring speed is 1500r/min;
and 5, mixing and washing the precipitate in the step 3 and the step 4, and drying to obtain calcium carbonate, wherein the washing adopts an ethanol water solution, the volume concentration of ethanol in the ethanol water solution is 75%, and the drying temperature is 110 ℃.
The average particle diameter of the nano calcium carbonate prepared in the embodiment is 500nm, wherein the particle content of 0-800nm is 91%, and the purity reaches 98.9%.
In summary, the invention has the following advantages:
1. the invention solves the problem of purity reduction caused by excessive auxiliary agents in the existing calcium carbonate technology, and realizes nano precipitation of calcium carbonate by utilizing the rapid conversion formed by different solubilities of calcium materials.
2. The invention uses the conversion of the solvent to control the dissolution change of the auxiliary agent, effectively solves the residual problem of the auxiliary agent, and improves the purity of the calcium carbonate.
3. The preparation method provided by the invention does not need high-temperature sintering, does not damage the chemical properties of raw materials, and can recycle the dispersing agent and the solvent.
4. The calcium carbonate prepared by the method has uniform particle size distribution and strong controllability, and shows good adsorptivity and stability in the field of material labels, so that the printing definition is improved, and the quality of the labels is greatly improved.
It is to be understood that the foregoing detailed description of the invention is merely illustrative of the invention and is not limited to the embodiments of the invention. It will be understood by those of ordinary skill in the art that the present invention may be modified or substituted for elements thereof to achieve the same technical effects; as long as the use requirement is met, the invention is within the protection scope of the invention.
Claims (1)
1. A method for preparing calcium carbonate, which is characterized in that: the method comprises the following steps:
step 1, adding calcium chloride into absolute ethyl alcohol, and stirring carboxymethyl cellulose and sodium dodecyl sulfate at constant temperature until the carboxymethyl cellulose and the sodium dodecyl sulfate are completely dissolved to obtain a dispersion suspension; the concentration of the calcium chloride in the absolute ethyl alcohol is 100-250g/L, the adding amount of the carboxymethyl cellulose is 30-50% of the mass of the calcium chloride, the adding amount of the sodium dodecyl sulfate is 5-10% of the mass of the calcium chloride, the constant temperature stirring temperature is 50-60 ℃, and the stirring speed is 1000-2000r/min;
step 2, spraying the dispersion suspension on a substrate, drying to obtain a mixed film, and repeating the operation for 10-200 times to obtain a mixed thick film; the spraying amount of the spray is 5-10g/cm 2 Spraying at 50-60deg.C and oven drying at 80-90deg.C;
step 3, placing the mixed thick film in a reaction kettle, placing the mixed thick film at the middle end of the reaction kettle, introducing n-amyl alcohol-water layering liquid at room temperature until the mixed thick film is completely settled, and filtering to obtain crystal precipitation; the room temperature is 10-20 ℃, the volume ratio of n-amyl alcohol to water in the layering liquid of n-amyl alcohol and water is 1:3-6, the mixed thick film is arranged in n-amyl alcohol, sodium carbonate is dissolved in water, and the adding amount of sodium carbonate is 100-120% of the mass of calcium chloride;
step 4, adding ethanol into the filtrate filtered in the step 3 and stirring uniformly until precipitation is no longer generated, and filtering to obtain secondary precipitation; the addition amount of the ethanol is 100-130% of the mass of the n-amyl alcohol, and the stirring speed is 1000-2000r/min;
and 5, mixing and washing the precipitate in the step 3 and the step 4, and drying to obtain calcium carbonate, wherein the washing adopts an ethanol water solution, the volume concentration of ethanol in the ethanol water solution is 70-80%, and the drying temperature is 100-120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011441604.1A CN112456532B (en) | 2020-12-08 | 2020-12-08 | Preparation method of calcium carbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011441604.1A CN112456532B (en) | 2020-12-08 | 2020-12-08 | Preparation method of calcium carbonate |
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| CN112456532A CN112456532A (en) | 2021-03-09 |
| CN112456532B true CN112456532B (en) | 2023-10-24 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585041A (en) * | 2016-01-26 | 2016-05-18 | 广西科技大学 | Preparation method of orange slice type calcium carbonate particles |
| CN109319815A (en) * | 2018-10-31 | 2019-02-12 | 吴亚良 | A kind of preparation method of nanometer calcium carbonate |
| CN111377477A (en) * | 2020-04-07 | 2020-07-07 | 绍兴文理学院 | Preparation method of nano titanium dioxide |
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2020
- 2020-12-08 CN CN202011441604.1A patent/CN112456532B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585041A (en) * | 2016-01-26 | 2016-05-18 | 广西科技大学 | Preparation method of orange slice type calcium carbonate particles |
| CN109319815A (en) * | 2018-10-31 | 2019-02-12 | 吴亚良 | A kind of preparation method of nanometer calcium carbonate |
| CN111377477A (en) * | 2020-04-07 | 2020-07-07 | 绍兴文理学院 | Preparation method of nano titanium dioxide |
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