CN100364892C - Process for preparing superfine dolomite - Google Patents

Process for preparing superfine dolomite Download PDF

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Publication number
CN100364892C
CN100364892C CNB2006100283580A CN200610028358A CN100364892C CN 100364892 C CN100364892 C CN 100364892C CN B2006100283580 A CNB2006100283580 A CN B2006100283580A CN 200610028358 A CN200610028358 A CN 200610028358A CN 100364892 C CN100364892 C CN 100364892C
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acid
dolomite
grinding aid
rhombspar
slurry
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CN1884081A (en
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施晓旦
王彦华
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Shanghai Dongsheng New Material Co Ltd
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Shanghai Dongsheng New Material Co Ltd
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Abstract

The present invention discloses a preparation method of superfine dolomite, which comprises the following steps: adding 300 to 350 meshes of dolomite powder and a grinding aid agent to water to prepare 45 to 75 wt% of superfine dolomite slurry; adopting a grinding device for the extra-fine grinding of dolomite to prepare superfine dolomite slurry, wherein the grinding aid agent is the esterification reaction product of dibasic acid and polyethylene glycol. The superfine dolomite prepared with the method of the present invention can be used as the pigment of paper coatings. The coating experiment by adopting superfine dolomite to replace 10 to 50% of ground limestone can prove that the indices, such as printing ink absorbability, brightness, printing brightness, wet repellence, etc. of finished paper products are much more increased than the original formulation.

Description

A kind of preparation method of super-fine dolomite
Technical field
The present invention relates to preparation method of super-fine dolomite.
Background technology
DOLOMITE CRYSTALS is rhombohedron, and is similar to the calcite crystal formation.Rhombspar has advantages such as impurity is few, whiteness is high, reserves are big, distribution is wide.At present rhombspar is mainly used in the raw material of introducing MgO in refractory materials, flux, the glass industry, preparation Magnesium Carbonate Light 41-45 etc.
The rhombspar of domestic production at present is generally tens to the hundreds of order, the thinnest 1000 orders that are no more than, thereby the application of rhombspar also is restricted.
The CN02136447.8 patent disclosure a kind of preparation method of super-fine dolomite, it is grinding aid that this patent adopts sodium polyacrylate or sodium phosphate, tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, therefore, the disclosed technology of this patent exists an obvious defects.The super fine bitter spar that it makes, median size are 1-2.5 μ m, and size range is wide, skewness, the slurry viscosity height of making, poor stability.
Summary of the invention:
The technical issues that need to address of the present invention are to disclose a kind of preparation method of super-fine dolomite, to overcome the above-mentioned defective that prior art exists.
Preparing method of super-fine dolomite of the present invention comprises the steps:
300~350 purpose ground dolomites and grinding aid are added in the entry, be made into weight content and be 45~75% super fine bitter spar slurry, adopt grinding plant that rhombspar is carried out ultra-fine mill then, make the super fine bitter spar slurry, wherein grain diameter is 60~100% less than the content of 2 μ m, and median size is 0.6~1.8 μ m.
The add-on of grinding aid is with respect to 0.1~5.0% of the weight of rhombspar dry powder.
Said grinding aid is the esterification reaction product of diprotic acid and polyoxyethylene glycol, and described diprotic acid is selected from one or more in oxalic acid, fumaric acid or the hexanodioic acid, and its molecular weight of described polyoxyethylene glycol can be 200-20000.
Grinding aid is to adopt following method to be prepared:
Diprotic acid and the polyoxyethylene glycol mole by 1: 1~1: 1.2 is mixed, be heated to 180~250 ℃ of esterifications then 3~5 hours, generate grinding aid diprotic acid list macrogol ester;
The molecular structure of grinding aid of the present invention is a long-chain, and an end of long-chain is a carboxyl, and it can be combined closely by chemical bond and dolomite particles surface; And the rest part of long chain molecule is a hydrophilic-structure, with water molecules good consistency is arranged, thereby the small-particle after the grinding is dispersed in the water well, has stoped intergranular reunion once more, guarantees that the super fine bitter spar size range that makes is narrow, is evenly distributed.
Described grinding plant is separate unit or many placed in-line machine or the stirring mills of delaminating.
The prepared super fine bitter spar of the present invention is used for paper making and cloth coating pigment.Replace the 10%--50% water-ground limestone with super fine bitter spar, do the coating experiment, the ink absorption of finished paper, glossiness, print gloss, indexs such as wet repulsion improve a lot than original formulation.
The prepared super fine bitter spar of the present invention can be used for paper making and cloth coating pigment, replace the 10%--50% water-ground limestone with super fine bitter spar, do the coating experiment, the ink absorption of finished paper, glossiness, print gloss, indexs such as wet repulsion improve a lot than original formulation.
Embodiment
Embodiment 1
With 9 kilograms of oxalic acid and 80 kilogram molecular weights is that 800 polyoxyethylene glycol is put into reactor, is heated to 200 ℃ then and carries out esterification, and when the water yield that generates reached 1.8 kilograms, reaction finished, and obtains about 87 kilograms of oxalic acid list macrogol ester.
With 325 order ground dolomite slurrying, ground dolomite is added in the entry, and Xiang Shuizhong adds above-mentioned oxalic acid list macrogol ester, wherein adding oxalic acid list macrogol ester is 0.3% with respect to the weight of rhombspar dry powder, stirs to make the grinding aid dissolving, is made into weight content and is 65% rhombspar slurry, fully stir, make slurry obtain good flowability, adopt the ultra-fine machine of delaminating of wet type of 80 liters of two series connection then, rhombspar is carried out ultra-fine mill.Make the super fine bitter spar slurry, wherein grain diameter is 90% less than the content of 2 μ m, and median size is 1.0 μ m.Adopt the method for ISO 2884-2-2003 standard code, recording slurry viscosity with NDJ-1 type rotational viscosimeter is 210 centipoises.
Super fine bitter spar with preparation replaces 50% water-ground limestone, does the coating experiment, and formulation for coating material sees Table 1.
Table 1
Coarse whiting Rhombspar China clay Calcined earth Whitening agent CMC Latex Plastic pigment
Original formulation % 36.81 0.00 48.88 11.28 0.45 0.60 14.29 3.00
Substitute prescription % 18.41 18.41 48.88 11.28 0.45 0.60 14.29 3.00
After coating prepared, be coated with, be coated on the blank cardboard and carry out, be coated with twice continuously with this coating, i.e. primary coat and in be coated with, glue spread is 18g/m 2Behind the letterweight light after the coating, adopt the GB/T1033-1995 standard to detect, detected result sees Table 2.
Table 2
Ink absorption % Glossiness % Absorption of inks speed Print gloss % Wet plucking % The wet % that repels
Original formulation 20.4 55.3 1.31 94 -0.9 21.1
Substitute prescription 23.3 59.6 1.07 97 -1.2 26.7
Embodiment 2
With 11.6 kilograms of fumaric acid and 20 kilogram molecular weights is that 200 polyoxyethylene glycol is put into reactor, is heated to 190 ℃ then and carries out esterification, and when the water yield that generates reached 1.8 kilograms, reaction finished, and obtains about 28 kilograms of fumaric acid list macrogol ester.
With 325 order ground dolomite slurrying, ground dolomite is added in the entry, and Xiang Shuizhong adds fumaric acid list macrogol ester, wherein adding fumaric acid list macrogol ester is 1.5% with respect to the weight of rhombspar dry powder, stirs to make the grinding aid dissolving, is made into weight content and is 75% rhombspar slurry, fully stir, make slurry obtain good flowability, adopt 300 liters the ultra-fine machine of delaminating of wet type then, rhombspar is carried out ultra-fine mill.Make the super fine bitter spar slurry, wherein less than 2 μ m content 98%, median size is 0.6 μ m.Adopt the method for ISO 2884-2-2003 standard code, recording slurry viscosity with NDJ-1 type rotational viscosimeter is 240 centipoises.
Super fine bitter spar with preparation replaces 40% water-ground limestone, does the coating experiment, and formulation for coating material sees Table 3.
Table 3
Coarse whiting Rhombspar China clay Calcined earth Whitening agent CMC Latex Plastic pigment
Original formulation % 36.81 0.00 48.88 11.28 0.45 0.60 14.29 3.00
Substitute prescription % 22.09 14.72 48.88 11.28 0.45 0.60 14.29 3.00
After coating prepared, be coated with, be coated on the blank cardboard and carry out, be coated with twice continuously with this coating, i.e. primary coat and in be coated with, glue spread is 18g/m 2Adopt the GB/T1033-1995 standard to detect behind the letterweight light after the coating, detected result sees Table 4.
Table 4
Ink absorption % Glossiness % Absorption of inks speed Print gloss % Wet plucking % The wet % that repels
Original formulation 20.4 55.3 1.31 94 -0.9 21.1
Substitute prescription 24.3 61.3 1.01 97 -1.5 27.3
Embodiment 3
With 1.46 kilograms of hexanodioic acids and 100 kilogram molecular weights is that 10000 polyoxyethylene glycol is put into reactor, is heated to 250 ℃ then and carries out esterification, and when the water yield that generates reached 0.2 kilogram, reaction finished, and obtains about 101 kilograms of hexanodioic acid list macrogol ester.
With 325 order ground dolomite slurrying, ground dolomite is added in the entry, and Xiang Shuizhong adds hexanodioic acid list macrogol ester, wherein adding hexanodioic acid list macrogol ester is 2.0% with respect to the weight of rhombspar dry powder, stirs to make the grinding aid dissolving, is made into weight content and is 60% rhombspar slurry, fully stir, make slurry obtain good flowability, adopt 3000 liters the ultra-fine machine of delaminating of wet type then, rhombspar was carried out ultra-fine mill 24 hours.Make the super fine bitter spar slurry, wherein less than 2 μ m content 95%, median size is 0.8 μ m.Adopt the method for ISO 2884-2-2003 standard code, recording slurry viscosity with NDJ-1 type rotational viscosimeter is 190 centipoises.
Super fine bitter spar with preparation replaces 30% water-ground limestone, does the coating experiment, and formulation for coating material sees Table 5.
Table 5
Coarse whiting Rhombspar China clay Calcined earth Whitening agent CMC Latex Plastic pigment
Original formulation % 36.81 0.00 48.88 11.28 0.45 0.60 14.29 3.00
Substitute prescription % 25.77 11.04 48.88 11.28 0.45 0.60 14.29 3.00
After coating prepared, be coated with, be coated on the blank cardboard and carry out, be coated with twice continuously with this coating, i.e. primary coat and in be coated with, glue spread is 18g/m 2Adopt the GB/T1033-1995 standard to detect behind the letterweight light after the coating, detected result sees Table 6.
Table 6
Ink absorption % Glossiness % Absorption of inks speed Print gloss % Wet plucking % The wet % that repels
Original formulation 20.4 55.3 1.31 94 -0.9 21.1
Substitute prescription 23.9 59.8 1.16 96 -1.1 28.0
Embodiment 4
With 9 kilograms of oxalic acid, 11.6 kilograms of fumaric acid and 80 kilogram molecular weights is that 400 polyoxyethylene glycol is put into reactor, be heated to 210 ℃ then and carry out esterification, when the water yield that generates reached 3.6 kilograms, reaction finished, and obtained about 97 kilograms of the sour single macrogol ester of oxalic acid richness/horse.
With 325 order ground dolomite slurrying, ground dolomite is added in the entry, and Xiang Shuizhong adds oxalic acid richness/single macrogol ester of horse acid, wherein adding the single macrogol ester of oxalic acid richness/horse acid is 1.3% with respect to the weight of rhombspar dry powder, stirs and makes the grinding aid dissolving, is made into weight content and is 70% rhombspar slurry, fully stir, make slurry obtain good flowability, adopt the ultra-fine machine of delaminating of wet type of 80 liters of three series connection then, rhombspar is carried out ultra-fine mill.Make the super fine bitter spar slurry, wherein less than 2 μ m content 96%, median size is 0.9 μ m.Adopt the method for ISO 2884-2-2003 standard code, recording slurry viscosity with NDJ-1 type rotational viscosimeter is 200 centipoises.
Super fine bitter spar with preparation replaces 50% water-ground limestone, does the coating experiment, and formulation for coating material sees Table 7.
Table 7
Coarse whiting Rhombspar China clay Calcined earth Whitening agent CMC Latex Plastic pigment
Original formulation % 36.81 0.00 48.88 11.28 0.45 0.60 14.29 3.00
Substitute prescription % 18.41 18.41 48.88 11.28 0.45 0.60 14.29 3.00
After coating prepared, be coated with, be coated on the blank cardboard and carry out, be coated with twice continuously with this coating, i.e. primary coat and in be coated with, glue spread is 18g/m 2Adopt the GB/T1033-1995 standard to detect behind the letterweight light after the coating, detected result sees Table 8.
Table 8
Ink absorption % Glossiness % Absorption of inks speed Print gloss % Wet plucking % The wet % that repels
Original formulation 20.4 55.3 1.31 94 -0.9 21.1
Substitute prescription 24.5 60.3 1.21 97 -1.7 28.1

Claims (5)

1. a preparation method of super-fine dolomite is characterized in that, comprises the steps:
300~350 purpose ground dolomites and grinding aid are added in the entry, be made into weight content and be 45~75% rhombspar slurry, adopt grinding plant that rhombspar is carried out ultra-fine mill then, make the super fine bitter spar slurry;
Said grinding aid is the esterification reaction product of diprotic acid and polyoxyethylene glycol;
Described diprotic acid is selected from one or more in oxalic acid, fumaric acid or the hexanodioic acid.
2. method according to claim 1 is characterized in that, its molecular weight of described polyoxyethylene glycol is 200-20000.
3. method according to claim 1 is characterized in that, the add-on of grinding aid is with respect to 0.1~5.0% of the weight of rhombspar dry powder.
4. method according to claim 1 is characterized in that, grinding aid is to adopt following method to be prepared:
With diprotic acid and polyoxyethylene glycol mixed in molar ratio by 1: 1~1: 1.2, be heated to 180~250 ℃ of esterifications then 3~5 hours, generate grinding aid diprotic acid list macrogol ester;
Described diprotic acid is selected from one or more in oxalic acid, fumaric acid or the hexanodioic acid;
Described polyoxyethylene glycol its minute suboutput is 200-20000.
5. method according to claim 1 is characterized in that, described grinding plant is separate unit or many placed in-line machine or the stirring mills of delaminating.
CNB2006100283580A 2006-06-29 2006-06-29 Process for preparing superfine dolomite Active CN100364892C (en)

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Publication number Priority date Publication date Assignee Title
WO2010008092A1 (en) * 2008-07-18 2010-01-21 花王株式会社 Method for producing hydraulic powder
CN107512741B (en) * 2017-09-04 2019-04-16 中国科学院地球化学研究所 A method of preparing ankerite at high temperature under high pressure

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1473783A (en) * 2002-08-09 2004-02-11 上海东升新材料有限公司 Process for preparing super fine bitter spar and use of super fine bitter spar
US20040198584A1 (en) * 2003-04-02 2004-10-07 Saint-Gobain Ceramics & Plastic, Inc. Nanoporous ultrafine alpha-alumina powders and freeze drying process of preparing same
CN1654585A (en) * 2005-01-17 2005-08-17 上海大学 Core/shell nano particle grinding agent polishing solution composition and method for preparing same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1473783A (en) * 2002-08-09 2004-02-11 上海东升新材料有限公司 Process for preparing super fine bitter spar and use of super fine bitter spar
US20040198584A1 (en) * 2003-04-02 2004-10-07 Saint-Gobain Ceramics & Plastic, Inc. Nanoporous ultrafine alpha-alumina powders and freeze drying process of preparing same
CN1654585A (en) * 2005-01-17 2005-08-17 上海大学 Core/shell nano particle grinding agent polishing solution composition and method for preparing same

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Denomination of invention: Process for preparing super fine bitter spar and use of super fine bitter spar

Effective date of registration: 20191225

Granted publication date: 20080130

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