CN108083313B - Preparation method of nano barium carbonate slurry - Google Patents
Preparation method of nano barium carbonate slurry Download PDFInfo
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- CN108083313B CN108083313B CN201810074795.9A CN201810074795A CN108083313B CN 108083313 B CN108083313 B CN 108083313B CN 201810074795 A CN201810074795 A CN 201810074795A CN 108083313 B CN108083313 B CN 108083313B
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- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 title claims abstract description 145
- 239000002002 slurry Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 35
- 239000004576 sand Substances 0.000 claims abstract description 26
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 18
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011324 bead Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 3
- 238000005086 pumping Methods 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 7
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 abstract description 40
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 12
- 239000012267 brine Substances 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 abstract description 12
- 229910001422 barium ion Inorganic materials 0.000 abstract description 6
- 239000011780 sodium chloride Substances 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 10
- 238000005259 measurement Methods 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 229910052736 halogen Inorganic materials 0.000 description 7
- 150000002367 halogens Chemical class 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052788 barium Inorganic materials 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FTYIWOBJJOVZLS-UHFFFAOYSA-L S(=O)(=O)([O-])[O-].[Ba+2].[Na+] Chemical compound S(=O)(=O)([O-])[O-].[Ba+2].[Na+] FTYIWOBJJOVZLS-UHFFFAOYSA-L 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
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
- C01F11/186—Strontium or barium carbonate
- C01F11/188—Barium carbonate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
Abstract
The invention discloses a preparation method of nano barium carbonate slurry, which comprises the steps of uniformly stirring barium carbonate with the average particle size of 1.0-8.0 mu m, deionized water and pentaerythritol or sodium polyacrylate, pumping the mixture to a ceramic horizontal sand mill by using a metering pump, adding zirconia beads with the particle size of 100-1200 mu m to grind the barium carbonate, controlling the flow rate of the metering pump at 3L/min, and controlling the rotation speed of the sand mill at 1450r/min to obtain the nano barium carbonate slurry. The nano barium carbonate slurry obtained by the invention can obviously improve the reaction rate of barium carbonate and sulfate radical during the preparation of the nano barium sulfate, can more effectively remove the sulfate radical in sodium chloride brine, effectively improve the use efficiency of the barium carbonate in the application of brine impurity removal, and the obtained nano barium carbonate is used as a raw material for preparing nano precipitated barium sulfate, so that the obtained nano precipitated barium sulfate powder has smaller particle size, and soluble barium ions and chloride ions are not detected by the nano precipitated barium sulfate powder.
Description
The technical field is as follows:
the invention relates to a preparation method of nano barium carbonate slurry.
Background art:
the nano barium carbonate is an important inorganic chemical product, barium sources for preparing the barium carbonate are barium chloride, barium hydroxide and the like, and carbon sources are mainly carbon dioxide (liquid state), carbonate (hydrogen) and the like; the existing preparation method comprises the following steps: reversed micelle method, liquid phase reaction controlled precipitation method and solid phase reaction method. However, when the nano barium carbonate slurry prepared by the prior art is used for preparing the nano barium sulfate, the reaction rate is low, the sulfate radicals in the sodium chloride brine can not be effectively removed, and the use efficiency in the application of brine impurity removal is low.
The invention content is as follows:
the invention aims to provide a preparation method of nano barium carbonate slurry, the nano barium carbonate slurry obtained by the method can obviously improve the reaction rate of barium carbonate and sulfate radicals during the preparation of sodium barium sulfate, can more effectively remove the sulfate radicals in sodium chloride brine, and effectively improve the use efficiency of barium carbonate in brine impurity removal application, the obtained nano barium carbonate is used as a raw material for preparing nano precipitated barium sulfate, the particle size of the obtained nano precipitated barium sulfate powder is smaller, and the nano precipitated barium sulfate powder cannot detect soluble barium ions and halogen chloride ions.
The invention is realized by the following technical scheme:
a method for preparing nano barium carbonate slurry comprises the following steps: uniformly stirring barium carbonate with the average particle size of 1.0-8.0 mu m, deionized water and pentaerythritol or sodium polyacrylate, wherein the mass ratio of barium carbonate to water to pentaerythritol or sodium polyacrylate is 50-100: 50-100: 1-5, sequentially pumping the barium carbonate slurry to a 1-4# ceramic horizontal sand mill arranged in series by using a metering pump, performing primary grinding on the barium carbonate slurry by using the 1# sand mill, performing secondary grinding on the barium carbonate slurry by using a 2# sand mill, performing tertiary grinding on the barium carbonate slurry by using a 3# sand mill, performing four-stage grinding on the barium carbonate slurry by using a 4# sand mill, adding zirconia beads with the bead particle size of 100-2000 mu m into the sand mill, wherein the zirconia beads with the particle size of 600-2000 mu m are added into the 1-2# sand mill, the zirconia beads with the particle size of 100-800 mu m are added into the 3-4# sand mill, controlling the flow rate of the metering pump at 2-5L/min, controlling the rotation speed of the sand mill at 500-2000r/min, and preparing the nano-grade barium carbonate slurry after four-stage grinding.
Preferably, the mass ratio of barium carbonate, water, pentaerythritol or sodium polyacrylate is 80-100: 80-100: 1-5, and the flow rate of the metering pump is controlled at 2-3L/min.
The invention also protects the nano barium carbonate slurry obtained by the preparation method and application thereof.
Particularly, the nano barium carbonate obtained by the invention is used as a raw material for preparing nano precipitated barium sulfate, the obtained nano precipitated barium sulfate powder has smaller particle size, and soluble barium ions and halogen chloride ions are not detected in the nano precipitated barium sulfate powder.
The invention has the following beneficial effects:
1) the nano barium carbonate slurry obtained by the invention can obviously improve the reaction rate of barium carbonate and sulfate radical during the preparation of the nano barium sulfate, can more effectively remove the sulfate radical in sodium chloride brine, and effectively improve the use efficiency of barium carbonate in the application of brine impurity removal.
2) The nano barium carbonate obtained by the invention is used as a raw material for preparing nano precipitated barium sulfate, the obtained nano precipitated barium sulfate powder has smaller particle size, and soluble barium ions and halogen chloride ions are not detected by the nano precipitated barium sulfate powder.
Description of the drawings:
FIG. 1 is a graph showing the results of particle size measurement of a nano-sized barium carbonate slurry obtained in example 1;
FIG. 2 is an SEM scanning electron micrograph of a nano-sized barium carbonate slurry obtained in example 1;
FIG. 3 shows the results of particle size measurement of the nano-sized barium carbonate slurry obtained in example 2;
FIG. 4 is a result of particle size measurement of the nano-sized barium carbonate slurry obtained in comparative example 1;
fig. 5 shows the results of particle size measurement of the nano-sized barium carbonate slurry obtained in comparative example 2.
FIG. 6 is a scanning electron microscope image of nano-precipitated barium sulfate prepared using the nano-barium carbonate slurry prepared in example 1 as a raw material.
The specific implementation mode is as follows:
the following is a further description of the invention and is not intended to be limiting.
Example 1:
100Kg of barium carbonate (light barium carbonate with the average particle size of 2.67 mu m produced by Guizhou Hongxing) is added into a 200L stainless steel stirring barrel, 100Kg of deionized water is added, 2 Kg of pentaerythritol is added, the mixture is uniformly stirred in the stainless steel stirring barrel, and then the mixture is sequentially pumped into a 10L serial 1-4# ceramic horizontal sand mill (a Palenian sand mill PHN-10) by a metering pump, zirconia beads (Zirmil Y produced by Stigobian Siepu) are added into the ceramic horizontal sand mill, wherein the particle size of the zirconia beads added into the 1-2# sand mill is 800-, and finally, four-stage grinding is carried out through a No. 4 sand mill, the flow rate of a metering pump is controlled at 3L/min, the rotation speed of the sand mill is 1450r/min, and nano-grade barium carbonate slurry can be prepared after four-stage grinding. The particle size measurement results are shown in FIG. 1, the average particle size is 98.2nm, and the SEM image is shown in FIG. 2.
Example 2:
referring to example 1, except that pentaerythritol was replaced with sodium polyacrylate, nano-sized barium carbonate slurry was prepared, and the result of particle size measurement was shown in fig. 3, with an average particle size of 96.6 nm.
Comparative example 1:
referring to example 1, except that pentaerythritol was replaced with sodium carbonate, a nano-scale barium carbonate slurry was prepared. The results of the particle size measurement are shown in FIG. 4, and the average particle size is 271.4 nm.
Comparative example 2:
reference example 1 with the exception that no pentaerythritol was added.
The results of particle size measurement of the obtained barium carbonate slurry are shown in FIG. 5, and the average particle size is 352.6 nm.
Example 3:
reference example 1, except that: the pentaerythritol content is 1 kg, and the flow rate of the metering pump is controlled at 2L/min.
Example 4:
reference example 1, except that: the pentaerythritol content is 10kg, and the flow rate of a metering pump is controlled at 5L/min.
Test detection example:
the barium carbonate slurries prepared in the above examples 1 to 4 and comparative examples 1 to 2 and commercially available light barium carbonate (light barium carbonate produced by red star development, Guizhou, having an average particle diameter of 2.67 μm) were respectively subjected to reactivity tests using the following methods:
1. adding 1000 ml of industrial sodium chloride brine into a 2000 ml glass beaker, adding 20G of the barium carbonate sample prepared in different examples 1-4 and comparative examples 1-2 in terms of solid content, keeping the solution at a constant temperature of 60 ℃, stirring for 30 minutes at a stirring speed of 200r/min, filtering by using a G4 sand core funnel, taking out a filtered clear solution, and detecting the sulfate radical content before and after the reaction of the brine and the barium carbonate.
2. Adding 500 ml of deionized water into a 1000 ml glass beaker, adding 100g of barium carbonate sample, stirring at a stirring speed controlled at 200r/min, adding 98% concentrated sulfuric acid at a stirring speed controlled at 5-10 g/min until the pH value is equal to 2 at the end of the reaction, recording the adding weight of the sulfuric acid, and finally calculating the reaction rate of barium carbonate and the sulfuric acid.
The test data are shown in table 1:
TABLE 1
From the experimental data in table 1, the nano barium carbonate of the present invention can significantly improve the reaction rate of the product and sulfate radicals, can more effectively remove the sulfate radicals in the sodium chloride brine, effectively improve the utilization efficiency of barium carbonate in the application of brine impurity removal, and can also greatly improve the reaction rate of barium carbonate and sulfuric acid.
3. 50Kg of deionized water was added to a 100L enamel reactor, 5Kg of concentrated sulfuric acid (concentration: 98%) was added thereto, the temperature was maintained at 45-55 deg.C, and 20Kg of the nano barium carbonate slurry (barium carbonate solid content: about 10Kg) prepared in the above example 1 or comparative example 1 or commercially available light barium carbonate (light barium carbonate produced by Hongxing, Guizhou, average particle size: 2.67 μm) was slowly pumped into the 100L enamel reactor by a metering pump for 10min until the barium carbonate reaction was completed. The pH value at the end of the reaction is controlled between 2.0 and 3.0. Stirring for 1 hour at constant temperature, and adjusting the pH value to 7-7.5 by using a 10% sodium hydroxide solution to obtain the nano precipitated barium sulfate slurry. Filtering, washing, drying and airflow crushing to obtain nanometer precipitated barium sulfate powder. The particle size measurement was carried out, and the average particle size of the nano-precipitated barium sulfate powder (shown in FIG. 6 by scanning electron microscope) prepared from the nano-barium carbonate slurry obtained in example 1 was 64.2nm, the average particle size of the nano-precipitated barium sulfate powder prepared from the nano-barium carbonate slurry obtained in comparative example 1 was 123nm, and the average particle size of the nano-precipitated barium sulfate powder prepared from commercially available light barium carbonate was 193 nm. The nano precipitated barium sulfate powder prepared above, and also commercially available nano precipitated barium sulfate (nano precipitated barium sulfate MB-103 produced by qingyuan, average particle size of 80nm) were mixed according to standard EN71Part 3:1994 and EN 14582: 2007 progressive testing of soluble barium (Ba) and halogen (chlorocl):
the test results are shown in table 2: (ND represents not detected)
TABLE 2
| Test items | Unit of | Example 1 | Comparative example 1 | MB-103 |
| Soluble barium (Ba) | mg/kg | ND | 1250 | 3590 |
| Halogen chlorine (Cl) | mg/kg | ND | ND | 650 |
The results show that the nano precipitated barium sulfate prepared by using the nano barium carbonate prepared by the invention can not detect soluble barium ions and halogen chloride ions, while the comparative samples have the problem of soluble barium ions and MB-103 also has the problem of halogen Cl.
Claims (2)
1. A preparation method of nano barium carbonate slurry is characterized by comprising the following steps: uniformly stirring barium carbonate with the average particle size of 1.0-8.0 mu m, deionized water and pentaerythritol, wherein the mass ratio of barium carbonate to water to pentaerythritol is 50-100: 50-100: 1-5, sequentially pumping the barium carbonate slurry to a 1-4# ceramic horizontal sand mill arranged in series by using a metering pump, performing primary grinding on the barium carbonate slurry by using the 1# sand mill, performing secondary grinding on the barium carbonate slurry by using a 2# sand mill, performing tertiary grinding on the barium carbonate slurry by using a 3# sand mill, performing four-stage grinding on the barium carbonate slurry by using a 4# sand mill, adding zirconia beads with the bead particle size of 100-2000 mu m into the sand mill, wherein the zirconia beads with the particle size of 600-2000 mu m are added into the 1-2# sand mill, the zirconia beads with the particle size of 100-800 mu m are added into the 3-4# sand mill, controlling the flow rate of the metering pump at 2-5L/min, controlling the rotation speed of the sand mill at 500-2000r/min, and preparing the nano-grade barium carbonate slurry after four-stage grinding.
2. The method for preparing nano barium carbonate slurry according to claim 1, wherein the mass ratio of barium carbonate, water and pentaerythritol is 80-100: 80-100: 1-5; the flow rate of the metering pump is controlled to be 2-3L/min.
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