CN116654967A - Preparation method of spherical nano barium carbonate easy for solid-liquid separation - Google Patents
Preparation method of spherical nano barium carbonate easy for solid-liquid separation Download PDFInfo
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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 188
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000007788 liquid Substances 0.000 title claims abstract description 34
- 238000000926 separation method Methods 0.000 title abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 72
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 48
- 239000008367 deionised water Substances 0.000 claims abstract description 43
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 43
- 239000013078 crystal Substances 0.000 claims abstract description 29
- 239000007787 solid Substances 0.000 claims abstract description 28
- 238000005054 agglomeration Methods 0.000 claims abstract description 27
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims abstract description 27
- 229910001626 barium chloride Inorganic materials 0.000 claims abstract description 27
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 239000004744 fabric Substances 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims description 26
- 239000000725 suspension Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 12
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 12
- 229920000858 Cyclodextrin Polymers 0.000 claims description 11
- 239000001116 FEMA 4028 Substances 0.000 claims description 11
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 11
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 11
- 229960004853 betadex Drugs 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 7
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 7
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 7
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 7
- 229920002401 polyacrylamide Polymers 0.000 claims description 7
- LXAHHHIGZXPRKQ-UHFFFAOYSA-N 5-fluoro-2-methylpyridine Chemical compound CC1=CC=C(F)C=N1 LXAHHHIGZXPRKQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 3
- 239000000693 micelle Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 159000000009 barium salts Chemical class 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- -1 enamel Substances 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 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
- C01F11/186—Strontium or barium carbonate
- C01F11/188—Barium carbonate
-
- 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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of spherical nano barium carbonate easy for solid-liquid separation, which comprises the following steps: (1) Dissolving barium chloride in deionized water to prepare a barium chloride solution, and then adding a crystal form control agent into the barium chloride solution to obtain a solution A; (2) Adding sodium carbonate into deionized water to prepare sodium carbonate solution, and then adding sodium dodecyl sulfate into the sodium carbonate solution to obtain solution B; (3) Slowly dripping the solution B into the solution A, regulating the pH of the solution, stirring for reaction after dripping, adding a micro-agglomeration agent after the reaction is completed, stirring uniformly, and then performing filter pressing by using filter cloth to obtain solid barium carbonate; (4) And washing, drying and ball-milling the solid barium carbonate to obtain the spherical nano barium carbonate. The invention can prepare spherical nano barium carbonate on one hand, and can separate solid from liquid through conventional filter cloth on the other hand, thereby having good industrial application prospect.
Description
Technical Field
The invention belongs to the technical field of inorganic nano materials, and particularly relates to a preparation method of spherical nano barium carbonate easy for solid-liquid separation.
Background
Barium carbonate is one of the important inorganic chemical products and also one of the most important barium salts. It is widely used in kinescope, accumulator, capacitor, ceramic, enamel, optical glass, pigment, paint, rubber, paint, ferrite, welding rod, water treatment, steel carburization, radio element, brick for high-rise building, barium salt manufacture, precursor material for preparing superconductor and ceramic material, etc.
In the field of electronic materials, barium carbonate is one of the most main raw materials for preparing dielectric materials in a multilayer ceramic capacitor (MLCC), along with the progress of technology and the increasing expansion of the application field of barium carbonate, and the trend of electronic products towards miniaturization, ultra-thinning and portability, corresponding MLCC also towards miniaturization and lamellar development, the raw materials for producing dielectric materials are required to be nano-sized, moreover, the quality requirements of enterprises on barium carbonate crystals are higher and higher, the preparation of barium carbonate powder with controllable morphology and size and uniform distribution becomes a current research hot spot, and the application of spherical barium carbonate in capacitors can effectively increase dielectric constant and improved temperature characteristics, so that the spherical barium carbonate has the characteristics of miniaturization, high frequency, large capacity and the like, and therefore, the research on a stable and feasible method for preparing spherical nano barium carbonate crystals has important significance.
However, in the preparation of ultrafine powder materials and nano powder materials, the current popular methods are aqueous phase chemical reduction method, sol-gel method and the like, and in the later process of the preparation of the methods, the solid-liquid separation process is encountered, and as the particle size of the powder particles is smaller and the surface energy is large, the powder particles can be suspended in liquid, so that the solid-liquid separation is difficult and the solid-liquid separation cannot be carried out by using conventional filter cloth filter pressing.
The Chinese patent application No. 20110126146. X discloses a solid-liquid separation method of superfine powder slurry, which comprises the following specific steps: firstly, placing the powder slurry in an environment of-50 ℃ to 0 ℃ for freezing until the powder slurry is completely frozen and is in a solid state; heating up and melting the frozen slurry, and standing for precipitation; after the standing precipitation is finished, directly pouring out the supernatant or discharging the supernatant through a valve on the container, thereby realizing solid-liquid separation. The powder particles form physical agglomerates in the freezing process, the properties and the surface morphology of the powder are not changed, and the particle size distribution of the powder can be kept unchanged after sedimentation; the drying cost of the powder material can be greatly reduced through solid-liquid separation; the powder material prepared by the separation method has better dispersibility. However, the solid-liquid separation method of the patent needs to be frozen at low temperature, has higher requirements on production equipment, has high energy consumption, improves the production cost and limits the industrial application of the method.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of spherical nano barium carbonate which is easy to separate solid from liquid.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the preparation method of the spherical nano barium carbonate easy for solid-liquid separation comprises the following steps:
(1) Dissolving barium chloride in deionized water to prepare a barium chloride solution with the concentration of 0.1-0.5mol/L, then adding a crystal form control agent into the barium chloride solution, and uniformly stirring to obtain a solution A;
(2) Adding sodium carbonate into deionized water to prepare sodium carbonate solution with the concentration of 0.1-0.5mol/L, then adding sodium dodecyl sulfate into the sodium carbonate solution, and uniformly stirring to obtain solution B;
(3) Slowly dripping the solution B in the step (2) into the solution A in the step (1), controlling the temperature to be 5-8 ℃, adding ammonia water to adjust the pH of the solution, stirring the solution after dripping is completed, obtaining a barium carbonate suspension after the reaction is completed, adding a micro-agglomeration agent into the barium carbonate suspension, stirring the solution for 0.5-1h at 40-50 ℃ and 60-80r/min, and then performing filter pressing by using filter cloth to obtain solid barium carbonate;
(4) And (3) washing, drying and ball-milling the solid barium carbonate in the step (3) to obtain the spherical nano barium carbonate.
Preferably, the preparation method of the crystal form control agent in the step (1) is as follows: adding beta-cyclodextrin into deionized water, stirring and dissolving, adding octadecyl trimethyl ammonium chloride and octyl phenol polyoxyethylene ether, stirring and reacting, and obtaining the crystal form control agent after the reaction is completed.
Preferably, the mass ratio of the beta-cyclodextrin to the deionized water to the octadecyl trimethyl ammonium chloride to the octyl phenol polyoxyethylene ether is 5:200-300:6-12:4-8; the temperature of the stirring reaction is 40-60 ℃, and the reaction time is 5-7h.
Preferably, the amount of the crystal form control agent added in the step (1) is 1 to 4wt% of the barium chloride solution.
Preferably, the sodium dodecyl sulfate in step (2) is added in an amount of 0.1 to 0.3wt% of the sodium carbonate solution.
Preferably, the preparation method of the micro-agglomeration agent in the step (3) comprises the following steps: adding 5-10g of polyacrylamide into 200mL of deionized water, stirring and dissolving, then adding 3-5g of hydroxypropyl cellulose and 1-3g of sodium lignin sulfonate, stirring and reacting for 2-4h at 50-60 ℃, and cooling after the reaction is finished to obtain the micro-agglomeration agent.
Preferably, the volume ratio of the solution A to the solution B in the step (3) is 1:1; the concentration of the ammonia water is 5-10wt%; the pH is 8-9; the dropping speed of the solution B is 600-800L/h; the temperature of the stirring reaction is 5-10 ℃, the stirring speed is 100-150r/min, and the reaction time is 1-2h.
Preferably, the addition amount of the micro-agglomeration agent in the step (3) is 0.01-0.03wt% of the barium carbonate suspension; the specification of the filter cloth is as follows: the mesh number is 600 meshes, and the gram weight is 100-150g/m 2 。
The addition amount of the micro-agglomeration agent is most suitable under the concentration, so that the nano barium carbonate can generate moderate agglomeration, the addition amount is too low, the agglomeration formed by the nano barium carbonate is too small, the solid-liquid separation is not easy to carry out, the addition amount is too high, and the agglomeration formed by the nano barium carbonate is too large, thereby being unfavorable for subsequent ball milling dispersion.
Preferably, the washing process in the step (4) is to wash with deionized water until the chloride ion content is less than 150ppm, then add EDTA disodium water solution with mass concentration of 1-3%, stir and soak for 40-60min, filter and then wash with deionized water until the chloride ion content is less than 30ppm; the temperature of the drying is 100-110 ℃, and the drying time is 3-4h.
The invention also protects the spherical nano barium carbonate prepared by the preparation method, the particle size of the spherical nano barium carbonate is less than or equal to 200nm, and the particle morphology is spherical or spheroidic.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the preparation method of the spherical nano barium carbonate easy to separate solid from liquid, beta-cyclodextrin, octadecyl trimethyl ammonium chloride and octyl phenol polyoxyethylene ether are subjected to self-assembly, hydrophobic alkyl chains in the octadecyl trimethyl ammonium chloride and the octyl phenol polyoxyethylene ether are inserted into cavities of the beta-cyclodextrin to form spherical micelles or vesicles, and then the spherical micelles or vesicles are added into a barium chloride solution as a crystal form control agent, and in the process of generating barium carbonate crystal grains, the growth in the linear direction is inhibited due to the influence of the spherical micelles and vesicles, so that the length-diameter ratio of the barium carbonate particles is reduced, spherical or spheroidal barium carbonate particles are gradually obtained, and meanwhile, the surface energy of the barium carbonate crystal grains in all directions can be changed by the octadecyl trimethyl ammonium chloride and the octyl phenol polyoxyethylene ether, so that the barium carbonate is dispersed more uniformly in the solution, and the obtained barium carbonate has smaller particle size; and by adding sodium dodecyl sulfate into the sodium carbonate solution, the formation of the barium carbonate particles into spheres or spheroids can be further controlled, and the sphericity rate of the barium carbonate particles is improved.
(2) According to the preparation method of the spherical nano barium carbonate easy to separate solid from liquid, the micro-agglomeration agent is added after the preparation of the barium carbonate suspension, so that the Zeta potential on the surface of the nano barium carbonate is reduced, micro-agglomeration of the nano barium carbonate is promoted, the particle size of the micro-agglomerated barium carbonate is increased and is not easy to permeate through filter cloth, the solid-liquid separation of the filter cloth in the subsequent step is facilitated, and the micro-agglomerated state of the filtered barium carbonate particles is destroyed through washing and ball milling, so that the nano spherical barium carbonate particles are obtained again.
(3) The spherical nano barium carbonate prepared by the method has the advantages of simple production process, concentrated particle size distribution, spherical or spheroidic morphology of nano barium carbonate and good application prospect.
Drawings
FIG. 1 is an SEM image of spherical nano barium carbonate prepared in example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The polyacrylamide is purchased from Xinxiang city Linglong water treatment materials limited company; the hydroxypropyl cellulose was purchased from atanan hong Xu chemical Co., ltd; the sodium lignin sulfonate is purchased from Jinan Chen Star chemical Co.
Example 1
The preparation method of the spherical nano barium carbonate easy for solid-liquid separation comprises the following steps:
(1) Dissolving barium chloride in deionized water to prepare a barium chloride solution with the concentration of 0.1mol/L, then adding 1wt% of a crystal form control agent into the barium chloride solution, and uniformly stirring to obtain a solution A;
(2) Adding sodium carbonate into deionized water to prepare a sodium carbonate solution with the concentration of 0.1mol/L, then adding 0.1wt% of sodium dodecyl sulfate into the sodium carbonate solution, and uniformly stirring to obtain a solution B;
(3) Slowly dropwise adding the solution B in the step (2) into the solution A in the step (1) at the dropwise adding speed of 600L/h, controlling the temperature at 8 ℃, adding 5wt% ammonia water to adjust the pH of the solution to 8, stirring the solution after the dropwise adding is completed, reacting at the temperature of 5 ℃ at the stirring speed of 100r/min for 2h, obtaining a barium carbonate suspension after the reaction is completed, adding 0.01wt% micro-agglomeration agent into the barium carbonate suspension, stirring the solution for 1h at the temperature of 40 ℃ at the speed of 60r/min, and then performing filter pressing by using filter cloth, wherein the specification of the filter cloth is as follows: the mesh number is 600 meshes, and the gram weight is 150g/m 2 Obtaining solid barium carbonate;
(4) Washing the solid barium carbonate in the step (3) with deionized water until the chloride ion content is less than 150ppm, then adding EDTA disodium water solution with the mass concentration of 1%, stirring and soaking for 40min, filtering, washing with deionized water until the chloride ion content is less than 30ppm, drying at 100 ℃ for 4h, and ball-milling to obtain the spherical nano barium carbonate.
The preparation method of the crystal form control agent comprises the following steps: adding 5g of beta-cyclodextrin into 250g of deionized water, stirring and dissolving, adding 9g of octadecyl trimethyl ammonium chloride and 6g of octyl phenol polyoxyethylene ether, stirring and reacting for 6h at 50 ℃, and obtaining the crystal form control agent after the reaction is completed.
The preparation method of the micro-agglomeration agent comprises the following steps: adding 5g of polyacrylamide into 200mL of deionized water, stirring and dissolving, then adding 3g of hydroxypropyl cellulose and 1g of sodium lignin sulfonate, stirring and reacting for 4 hours at 50 ℃, and cooling after the reaction is completed, thus obtaining the micro-agglomeration agent.
As shown in FIG. 1, the spherical nano barium carbonate particles prepared in the embodiment are spherical or spheroid, and the average particle size is 137nm.
Example 2
The preparation method of the spherical nano barium carbonate easy for solid-liquid separation comprises the following steps:
(1) Dissolving barium chloride in deionized water to prepare a barium chloride solution with the concentration of 0.3mol/L, then adding 2wt% of a crystal form control agent into the barium chloride solution, and uniformly stirring to obtain a solution A;
(2) Adding sodium carbonate into deionized water to prepare a sodium carbonate solution with the concentration of 0.3mol/L, then adding 0.2wt% of sodium dodecyl sulfate into the sodium carbonate solution, and uniformly stirring to obtain a solution B;
(3) Slowly dropwise adding the solution B in the step (2) into the solution A in the step (1) at the dropwise adding speed of 700L/h, controlling the temperature at 6 ℃, adding 7wt% ammonia water to adjust the pH of the solution to 8, stirring the solution after the dropwise adding is completed, reacting at the temperature of 7 ℃, the stirring speed of 120r/min, the reaction time of 2h, obtaining a barium carbonate suspension after the reaction is completed, adding 0.02wt% micro-agglomeration agent into the barium carbonate suspension, stirring the solution for 0.5h at 45 ℃ and 70r/min, and then performing filter pressing by using filter cloth with the specification of: the mesh number is 600 meshes, and the gram weight is 120g/m 2 Obtaining solid barium carbonate;
(4) Washing the solid barium carbonate in the step (3) with deionized water until the chloride ion content is less than 150ppm, then adding EDTA disodium water solution with the mass concentration of 2%, stirring and soaking for 50min, filtering, washing with deionized water until the chloride ion content is less than 30ppm, drying at 105 ℃ for 4h, and ball-milling to obtain the spherical nano barium carbonate.
The preparation method of the crystal form control agent comprises the following steps: adding 5g of beta-cyclodextrin into 250g of deionized water, stirring and dissolving, adding 9g of octadecyl trimethyl ammonium chloride and 6g of octyl phenol polyoxyethylene ether, stirring and reacting for 6h at 50 ℃, and obtaining the crystal form control agent after the reaction is completed.
The preparation method of the micro-agglomeration agent comprises the following steps: adding 7g of polyacrylamide into 200mL of deionized water, stirring and dissolving, then adding 4g of hydroxypropyl cellulose and 2g of sodium lignin sulfonate, stirring and reacting for 3 hours at 55 ℃, and cooling after the reaction is completed, thus obtaining the micro-agglomeration agent.
The spherical nano barium carbonate particles prepared in the embodiment are spherical or spheroid, and the average particle size is 153nm.
Example 3
The preparation method of the spherical nano barium carbonate easy for solid-liquid separation comprises the following steps:
(1) Dissolving barium chloride in deionized water to prepare a barium chloride solution with the concentration of 0.4mol/L, then adding 3wt% of a crystal form control agent into the barium chloride solution, and uniformly stirring to obtain a solution A;
(2) Adding sodium carbonate into deionized water to prepare a sodium carbonate solution with the concentration of 0.4mol/L, then adding 0.2wt% of sodium dodecyl sulfate into the sodium carbonate solution, and uniformly stirring to obtain a solution B;
(3) Slowly dropwise adding the solution B in the step (2) into the solution A in the step (1) at the dropwise adding speed of 700L/h, controlling the temperature at 7 ℃, adding 8wt% ammonia water to adjust the pH of the solution to 9, stirring the solution after the dropwise adding is completed, reacting at the temperature of 8 ℃, the stirring speed of 130r/min, the reaction time of 1.5h, obtaining a barium carbonate suspension after the reaction is completed, adding 0.02wt% micro-agglomeration agent into the barium carbonate suspension, stirring the solution for 0.5h at 45 ℃ and 70r/min, and then performing filter pressing by using filter cloth, wherein the specification of the filter cloth is as follows: the mesh number is 600 meshes, and the gram weight is 130g/m 2 Obtaining solid barium carbonate;
(4) Washing the solid barium carbonate in the step (3) with deionized water until the chloride ion content is less than 150ppm, then adding EDTA disodium water solution with the mass concentration of 2%, stirring and soaking for 50min, filtering, washing with deionized water until the chloride ion content is less than 30ppm, drying at 105 ℃ for 3.5h, and ball-milling to obtain the spherical nano barium carbonate.
The preparation method of the crystal form control agent comprises the following steps: adding 5g of beta-cyclodextrin into 250g of deionized water, stirring and dissolving, adding 9g of octadecyl trimethyl ammonium chloride and 6g of octyl phenol polyoxyethylene ether, stirring and reacting for 6h at 50 ℃, and obtaining the crystal form control agent after the reaction is completed.
The preparation method of the micro-agglomeration agent comprises the following steps: adding 8g of polyacrylamide into 200mL of deionized water, stirring and dissolving, then adding 4g of hydroxypropyl cellulose and 2g of sodium lignin sulfonate, stirring and reacting for 3 hours at 55 ℃, and cooling after the reaction is completed, thus obtaining the micro-agglomeration agent.
The spherical nano barium carbonate particles prepared in the embodiment are spherical or spheroid, and the average particle size is 161nm.
Example 4
The preparation method of the spherical nano barium carbonate easy for solid-liquid separation comprises the following steps:
(1) Dissolving barium chloride in deionized water to prepare a barium chloride solution with the concentration of 0.5mol/L, then adding 4wt% of a crystal form control agent into the barium chloride solution, and uniformly stirring to obtain a solution A;
(2) Adding sodium carbonate into deionized water to prepare a sodium carbonate solution with the concentration of 0.5mol/L, then adding 0.3wt% of sodium dodecyl sulfate into the sodium carbonate solution, and uniformly stirring to obtain a solution B;
(3) Slowly dropwise adding the solution B in the step (2) into the solution A in the step (1) at the dropwise adding speed of 800L/h, controlling the temperature at 5 ℃, adding 10wt% ammonia water to adjust the pH of the solution to 9, stirring the solution after the dropwise adding is completed, reacting at the temperature of 10 ℃, the stirring speed of 150r/min, reacting for 1h, obtaining a barium carbonate suspension after the reaction is completed, adding 0.03wt% micro-agglomeration agent into the barium carbonate suspension, stirring for 0.5h at the temperature of 50 ℃ and 80r/min, and then performing filter pressing by using filter cloth with the specification of: the mesh number is 600 meshes, and the gram weight is 100g/m 2 Obtaining solid barium carbonate;
(4) Washing the solid barium carbonate in the step (3) with deionized water until the chloride ion content is less than 150ppm, then adding EDTA disodium water solution with the mass concentration of 3%, stirring and soaking for 60min, filtering, washing with deionized water until the chloride ion content is less than 30ppm, drying at 110 ℃ for 3h, and ball-milling to obtain the spherical nano barium carbonate.
The preparation method of the crystal form control agent comprises the following steps: adding 5g of beta-cyclodextrin into 250g of deionized water, stirring and dissolving, adding 9g of octadecyl trimethyl ammonium chloride and 6g of octyl phenol polyoxyethylene ether, stirring and reacting for 6h at 50 ℃, and obtaining the crystal form control agent after the reaction is completed.
The preparation method of the micro-agglomeration agent comprises the following steps: adding 10g of polyacrylamide into 200mL of deionized water, stirring and dissolving, then adding 5g of hydroxypropyl cellulose and 3g of sodium lignin sulfonate, stirring and reacting for 2 hours at 60 ℃, and cooling after the reaction is completed, thus obtaining the micro-agglomeration agent.
The spherical nano barium carbonate particles prepared in the embodiment are spherical or spheroid, and the average particle size is 185nm.
Comparative example 1
The preparation method of the spherical nano barium carbonate easy for solid-liquid separation comprises the following steps:
(1) Dissolving barium chloride in deionized water to prepare a barium chloride solution with the concentration of 0.1mol/L, then adding 1wt% of a crystal form control agent into the barium chloride solution, and uniformly stirring to obtain a solution A;
(2) Adding sodium carbonate into deionized water to prepare a sodium carbonate solution with the concentration of 0.1mol/L, then adding 0.1wt% of sodium dodecyl sulfate into the sodium carbonate solution, and uniformly stirring to obtain a solution B;
(3) Slowly dropwise adding the solution B in the step (2) into the solution A in the step (1) at the dropwise adding speed of 600L/h, controlling the temperature at 8 ℃, adding 5wt% ammonia water to adjust the pH of the solution to 8, stirring the solution after the dropwise adding is completed, reacting at the temperature of 5 ℃ at the stirring speed of 100r/min for 2h, obtaining a barium carbonate suspension after the reaction is completed, and then performing filter pressing by using filter cloth with the specification of: the mesh number is 600 meshes, and the gram weight is 150g/m 2 The filter cloth cannot perform solid-liquid separation.
The preparation method of the crystal form control agent comprises the following steps: adding 5g of beta-cyclodextrin into 250g of deionized water, stirring and dissolving, adding 9g of octadecyl trimethyl ammonium chloride and 6g of octyl phenol polyoxyethylene ether, stirring and reacting for 6h at 50 ℃, and obtaining the crystal form control agent after the reaction is completed.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the spherical nano barium carbonate easy to separate solid from liquid is characterized by comprising the following steps of:
(1) Dissolving barium chloride in deionized water to prepare a barium chloride solution with the concentration of 0.1-0.5mol/L, then adding a crystal form control agent into the barium chloride solution, and uniformly stirring to obtain a solution A;
(2) Adding sodium carbonate into deionized water to prepare sodium carbonate solution with the concentration of 0.1-0.5mol/L, then adding sodium dodecyl sulfate into the sodium carbonate solution, and uniformly stirring to obtain solution B;
(3) Slowly dripping the solution B in the step (2) into the solution A in the step (1), controlling the temperature to be 5-8 ℃, adding ammonia water to adjust the pH of the solution, stirring the solution after dripping is completed, obtaining a barium carbonate suspension after the reaction is completed, adding a micro-agglomeration agent into the barium carbonate suspension, stirring the solution for 0.5-1h at 40-50 ℃ and 60-80r/min, and then performing filter pressing by using filter cloth to obtain solid barium carbonate;
(4) And (3) washing, drying and ball-milling the solid barium carbonate in the step (3) to obtain the spherical nano barium carbonate.
2. The method for preparing spherical nano barium carbonate easy to separate solid from liquid according to claim 1, wherein the preparation method of the crystal form control agent in the step (1) is as follows: adding beta-cyclodextrin into deionized water, stirring and dissolving, adding octadecyl trimethyl ammonium chloride and octyl phenol polyoxyethylene ether, stirring and reacting, and obtaining the crystal form control agent after the reaction is completed.
3. The preparation method of the spherical nano barium carbonate easy to separate solid from liquid according to claim 2, wherein the mass ratio of the beta-cyclodextrin to the deionized water to the octadecyl trimethyl ammonium chloride to the octyl phenol polyoxyethylene ether is 5:200-300:6-12:4-8; the temperature of the stirring reaction is 40-60 ℃, and the reaction time is 5-7h.
4. The method for preparing spherical nano barium carbonate easy to separate solid and liquid according to claim 2, wherein the addition amount of the crystal form control agent in the step (1) is 1-4wt% of the barium chloride solution.
5. The method for preparing spherical nano barium carbonate easy to separate solid and liquid according to claim 1, wherein the adding amount of sodium dodecyl sulfate in the step (2) is 0.1-0.3wt% of sodium carbonate solution.
6. The method for preparing spherical nano barium carbonate easy to separate solid from liquid according to claim 1, wherein the preparation method of the micro-agglomeration agent in the step (3) is as follows: adding 5-10g of polyacrylamide into 200mL of deionized water, stirring and dissolving, then adding 3-5g of hydroxypropyl cellulose and 1-3g of sodium lignin sulfonate, stirring and reacting for 2-4h at 50-60 ℃, and cooling after the reaction is finished to obtain the micro-agglomeration agent.
7. The method for preparing spherical nano barium carbonate easy to separate solid from liquid according to claim 1, wherein the volume ratio of the solution A to the solution B in the step (3) is 1:1; the concentration of the ammonia water is 5-10wt%; the pH is 8-9; the dropping speed of the solution B is 600-800L/h; the temperature of the stirring reaction is 5-10 ℃, the stirring speed is 100-150r/min, and the reaction time is 1-2h.
8. The method for preparing spherical nano barium carbonate easy to separate solid and liquid according to claim 1, wherein the addition amount of the micro-agglomeration agent in the step (3) is 0.01-0.03wt% of the barium carbonate suspension; the specification of the filter cloth is as follows: the mesh number is 600 meshes, and the gram weight is 100-150g/m 2 。
9. The preparation method of the spherical nano barium carbonate easy to separate solid from liquid according to claim 1, wherein the washing process in the step (4) is to wash with deionized water until the chloride ion content is less than 150ppm, then adding EDTA disodium water solution with the mass concentration of 1-3%, stirring and soaking for 40-60min, filtering, and then washing with deionized water until the chloride ion content is less than 30ppm; the temperature of the drying is 100-110 ℃, and the drying time is 3-4h.
10. The spherical nano barium carbonate prepared by the preparation method according to any one of claims 1 to 9, wherein the particle size of the spherical nano barium carbonate is less than or equal to 200nm, and the morphology of the particles is spherical or spheroid.
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| CN117509718B (en) * | 2023-12-13 | 2024-05-28 | 湖北展鹏电子材料有限公司 | Spherical-like nano barium titanate and preparation method thereof |
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