CN112516928A - Solid sol preparation device and preparation method - Google Patents
Solid sol preparation device and preparation method Download PDFInfo
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- CN112516928A CN112516928A CN202011459366.7A CN202011459366A CN112516928A CN 112516928 A CN112516928 A CN 112516928A CN 202011459366 A CN202011459366 A CN 202011459366A CN 112516928 A CN112516928 A CN 112516928A
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- 239000008281 solid sol Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 64
- 238000003756 stirring Methods 0.000 claims abstract description 33
- 239000007921 spray Substances 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000007599 discharging Methods 0.000 claims abstract description 17
- 238000005507 spraying Methods 0.000 claims description 28
- 239000002270 dispersing agent Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 235000002639 sodium chloride Nutrition 0.000 claims description 10
- 239000008346 aqueous phase Substances 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 229910021645 metal ion Inorganic materials 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 6
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 6
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 230000014759 maintenance of location Effects 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 239000012716 precipitator Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 150000007942 carboxylates Chemical class 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 238000010008 shearing Methods 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- -1 sulfate ester salt Chemical class 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 3
- 229920000103 Expandable microsphere Polymers 0.000 description 14
- 230000006872 improvement Effects 0.000 description 9
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 9
- 239000000347 magnesium hydroxide Substances 0.000 description 9
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 9
- 229910000000 metal hydroxide Inorganic materials 0.000 description 8
- 150000004692 metal hydroxides Chemical class 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- 238000010557 suspension polymerization reaction Methods 0.000 description 8
- 229910001385 heavy metal Inorganic materials 0.000 description 7
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 6
- 239000001095 magnesium carbonate Substances 0.000 description 6
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- CADZRPOVAQTAME-UHFFFAOYSA-L calcium;hydroxy phosphate Chemical compound [Ca+2].OOP([O-])([O-])=O CADZRPOVAQTAME-UHFFFAOYSA-L 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 2
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 235000014413 iron hydroxide Nutrition 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 229910052621 halloysite Inorganic materials 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/11—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
- B01D29/31—Self-supporting filtering elements
- B01D29/35—Self-supporting filtering elements arranged for outward flow filtration
- B01D29/356—Self-supporting filtering elements arranged for outward flow filtration open-ended, the arrival of the mixture to be filtered and the discharge of the concentrated mixture are situated on both opposite sides of the filtering element
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Colloid Chemistry (AREA)
Abstract
The invention provides a preparation device and a preparation method of solid sol, wherein the preparation device of the solid sol comprises the following steps: (1) an electric device; (2) a spray assembly comprising one or more than one spray device, the spray device comprising in longitudinal order: a feeding pipe, a spray head and spray holes; (3) the reaction kettle comprises a sol detention area, the bottom of the reaction kettle is provided with a discharging bottom valve, and the discharging bottom valve is communicated with the sol detention area; (4) the porous screen is arranged in the reaction kettle, is provided with a plurality of screen holes and is communicated with the sol detention zone; (5) the stirring paddle is connected with the electric device, and the electric device controls the rotating speed of the stirring paddle. The invention also provides a preparation method of the solid sol, which solves the problem of poor dispersibility in the preparation of the solid sol, and can realize the preparation of the solid sol with certain particle size distribution by controlling the aperture size of the porous screen.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a solid sol preparation device and a preparation method.
Background
The metal hydroxide sol is mainly used for the adsorption of metal ions in wastewater treatment and an inorganic nano dispersant in suspension polymerization due to the special structure and good dispersibility of the metal hydroxide sol.
Firstly, the traditional method for treating the industrial wastewater containing heavy metal ions is roughly divided into two types, one type belongs to a chemical precipitation method; heavy metal ions in the wastewater are converted into insoluble metal compounds through double decomposition reaction, and are subjected to flocculation precipitation such as sodium polyacrylate and the like, so that the method for treating heavy metal ion pollution which is generally adopted at present is also adopted; one is physical adsorption; the heavy metal is concentrated and separated under the condition of not changing the chemical form of the heavy metal, mainly through adsorption treatment by an adsorption material, and the physical change is the main point. Because the chemical method has the defects of equipment corrosion, easy scaling and the like, the method for treating heavy metal pollution by the chemical method faces new challenges, people pay attention to the method for treating metal ions in wastewater by using the physical adsorption method in recent years, and the metal hydroxide solid sol is non-toxic and harmless, has large specific surface area and strong active adsorption capacity, and is easy to adsorb and remove Al which causes harm to the environment from various industrial waste liquids3+、Cd2+、Cu2+、Cr3+And (3) heavy metal ions.
Secondly, in the field of suspension polymerization, metal solid sols represented by magnesium hydroxide and calcium hydroxy phosphate have been successfully applied to the preparation of polyvinyl chloride, foamable styrene plastics, acrylonitrile suspension polymerization, expandable microspheres and the like. The surface of the metal solid sol is always adsorbed with more metal ions, and the metal solid sol and an anionic surfactant generate charge action, so that the hydrophilic metal solid sol is transferred to an oil-water interface to wrap emulsion formed by suspension polymerization, a mechanical isolation effect is achieved, and stable Pickering emulsion is formed, thereby ensuring that the suspension polymerization based on the Pickering emulsion can be realized.
The sol sold in the market at present is mainly silicon dioxide sol, commonly called as silica sol, has good dispersity when the particle size is 7-10nm, can form a firm and flat surface after being dried, and is mainly used in the coating industry. Secondly, in the field of expandable microsphere preparation, due to its good hydrophilicity and stability, it is usually used for preparing a stable aqueous suspension polymerization phase.
CN207102562U provides a simple operation, the high for chemistry iron hydroxide colloid preparation facilities of factor of safety, and this device has designed one kind and has utilized heating such as alcohol, through the operation form of slide linkage, has designed a simple and convenient iron hydroxide colloid preparation facilities, but this device operation is complicated, is difficult to carry out large-scale production preparation, receives the influence of used material form, is difficult to carry out the preparation of diversified solid sol.
CN209476119U is through all being fixed with the electric heat pole in the inside of a plurality of puddlers, can be for the electric heat pole circular telegram when the nanometer colloid raw materials of stirring, will heat it to make the puddler heat the nanometer colloid raw materials all the time when stirring the raw materials, thereby guarantee that the raw materials can be intensive mixing under hotter environment, but equipment is complicated, and the heating also can lead to being difficult to of particle diameter in the sol preparation in addition to control, and equipment practicality is lower.
CN207838765U drives the air guide rod through agitator motor and stirs, then blows off gaseous hole through blockking the fine hair cover panel to blow through gaseous in solution, increase the stirring effect of solution, though this equipment can increase stirring effect, but in the sol preparation, the air guide rod blocks up with keeping off fine hair cover panel easily, and equipment is difficult clean.
US3615972, first reported the synthesis of expandable microspheres, wherein the specific role of the solid sol in the preparation of expandable microspheres is detailed, based on the dual role of protection/isolation and lowering interfacial tension/improving dispersibility of the solid sol, the performance of different microspheres prepared by magnesium hydroxide and silica sol is compared, the preparation of the silica sol for expandable microspheres is mature, however, the reports of the metal hydroxide solid sol represented by magnesium hydroxide in the preparation of microspheres are very few, the magnesium hydroxide in the preparation of expandable microspheres has the advantages of being capable of being removed from the microsphere products and improving the product quality, the production of suspension polymerization by using the solid sol such as magnesium hydroxide is very few in the world at present, and no clear preparation method exists, but has important significance for products with huge economic value, such as expandable microspheres and the like.
The metal hydroxide sol preparation device provided by the invention aims at further expanding the synthesis method of the metal hydroxide sol, provides a solid sol for large-scale application, and has important significance for expandable microspheres and other suspension polymerization researches.
Disclosure of Invention
The invention aims to provide a solid sol preparation device and a preparation method, and provides a simple solid sol preparation device.
The technical scheme of the invention is realized as follows:
the invention provides a solid sol preparation device, comprising:
(1) the reaction kettle comprises a sol detention area, the bottom of the reaction kettle is provided with a discharging bottom valve, and the discharging bottom valve is communicated with the sol detention area;
(2) spray assembly evenly sets up at the reation kettle top, includes two or more spray set, spray set includes in proper order on vertical: a feeding pipe, a spray head and spray holes; the spray holes are detachably connected with the spray head, and the size of the spray holes can be selected. The spraying flow rate is controlled by the size of the spray holes and the flow rate of the feeding pipe. As a further improvement of the invention, the spray head is detachably connected with the feeding pipe. The feed pipe is inserted at the top of the reaction kettle. (3) The porous screen is arranged in the reaction kettle, is provided with a plurality of screen holes and is communicated with the sol detention zone; the porous screen is a screen with screen holes woven by stainless steel metal, and the size of the screen holes on the porous screen is between 100 and 1000 meshes. The porous screen is detachably connected with the inner wall of the reaction kettle, so that the cleaning is convenient.
(4) The stirring paddle is arranged in the reaction kettle. And the electric device is connected with the stirring paddle and controls the rotating speed of the stirring paddle.
As a further improvement of the invention, the stirring paddle is connected with an electric device for driving the stirring paddle to rotate.
The invention further provides a preparation method of the solid sol by using the device, which comprises the following steps:
s1, feeding: respectively preparing the precipitating agents into water phases, dropwise adding the water phases by the spraying device, forming sol inside the porous screen after the precipitating agents are contacted with each other, and enabling the sol to enter a sol retention area through the porous screen;
s2, dispersing: after the contact of the precipitator, the electric device drives the stirring paddle to carry out shearing dispersion;
s3, discharging: and discharging the solid sol positioned in the sol detention area through the discharging bottom valve.
As a further improvement of the invention, the precipitant comprises a precipitant 1 and a precipitant 2, wherein the precipitant 1 is selected from one or a combination of several of sodium hydroxide, potassium hydroxide, ammonia water, sodium carbonate and sodium bicarbonate; the precipitant 2 is Mg2 +、Al3+、Ca2+、Ba2+、Fe2+、Fe3+One or more soluble salts of metal ions in (a).
The main function of the precipitant 1 in the present invention is to provide OH-The main function of the radical, precipitant 2, is to provide MR+A group.
As a further improvement of the invention, the content of the precipitant 1 is 5 to 50 wt%, preferably 10 to 30 wt%, more preferably 10 to 20 wt% of the aqueous phase; the content of the precipitant 2 is 5 to 50 wt%, preferably 10 to 30 wt%, more preferably 10 to 20 wt% of the aqueous phase.
As a further improvement of the invention, in the step S1, a dispersant is further added in the feeding process, the addition amount of the dispersant is 0.01-5 wt%, preferably 0.1-5 wt%, and more preferably 1-3 t% of the water phase, and the dispersant is selected from one or a mixture of several of ionic, nonionic and polymeric dispersants.
As a further improvement of the invention, the dispersant is an anionic dispersant and is selected from one or a combination of more of sodium oleate, carboxylate, sulfate ester salt and sulfonate.
According to the invention, a certain amount of dispersant is added into the precipitator 1 or the precipitator 2, the dispersant can promote the adsorption of solid sol on the interface of oil drops, the dispersant can be ionic type, nonionic type, polymer type and other dispersants, the invention uses salt containing metal ions, the metal salt is generally hydrophilic, in order to increase the migration of the sol to the oil-water interface, the anionic dispersant is preferably used, the anionic dispersant and the metal ions form stable ionic bonds, and the stable adsorption of the sol on the oil drops is maintained to the maximum extent.
As a further improvement of the present invention, inorganic salts are also added during the feeding in step S1 in an amount of 0.5 to 50 wt%, preferably 1 to 30 wt%, more preferably 1 to 20 wt% of the aqueous phase.
The inorganic salt can keep the Zeta potential of the sol, generally, the Zeta potential for keeping the dispersibility of the solid sol is more than +/-30 mV, and the isoelectric point (Zeta is 0mV) of the solid sol moves towards the direction of increasing pH; thereby changing the dispersion stability of the sol.
As a further improvement of the invention, the inorganic salt is selected from one or a combination of several of sodium chloride, potassium chloride, magnesium sulfate and aluminum chloride.
As a further development of the invention, the solids content of the discharged solid sol in step S3 is 0 to 10%, preferably 0 to 5%.
The solid sol of the invention mainly refers to metal hydroxide sol, but is not limited to metal hydroxide sol, and can also be extended to the preparation of magnesium carbonate, calcium phosphate and halloysite nanotubes. In order to maintain good dispersibility, the solid sol generally has a solids content of from 0 to 10%, preferably from 0 to 5%, more preferably from 1 to 4%.
The invention further protects the solid sol prepared by the preparation method.
The invention has the following beneficial effects: the invention provides a simple device for preparing solid sol, which can prepare and obtain the uniformly dispersed solid sol by using a porous spray head and a porous screen, solves the problems of complex equipment and small production scale in the preparation of the solid sol, realizes the continuous preparation of the solid sol, and can effectively increase the dispersibility of the sol, improve the production efficiency and simultaneously achieve the purposes of energy conservation and environmental protection.
The invention also provides a method for jointly spraying and dripping, which solves the problem of poor dispersibility in the preparation of the solid sol, can realize the preparation of the solid sol with certain particle size distribution by controlling the aperture size of the porous screen, can successfully use the prepared solid sol for the preparation of the expandable microspheres, improves the reliability and the simplicity of the preparation of the solid sol, effectively improves the operation efficiency, is convenient to process, has low cost and is beneficial to realizing mass production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic view showing the construction of a solid sol preparing apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of a porous screen apparatus according to one embodiment of the present invention;
FIG. 3 is a schematic structural view of a spray device according to an embodiment of the present invention;
wherein, 100: a discharging bottom valve; 200: a sol hold-up zone; 300: a porous screen; 301: screening holes; 400: a spraying device; 401: a spray head; 402: spraying a hole; 403: a feed pipe; 500: an electric device; 600: and (4) a stirring paddle.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention provides a solid sol preparation apparatus, as shown in fig. 1, providing a solid sol preparation system, comprising:
(1) the electric-powered device (500) is provided with a power supply,
(2) spray device 400, spray device includes in order vertically: a feeding pipe 403, a spray head 401 and spray holes 402;
wherein the feeding pipe 403, the spray head 401 and the spray holes 402 form a spraying device;
wherein, the spraying device is composed of a spraying device 1 and a spraying device 2; the spraying device 1 has the same structure as the spraying device, and only one of the spraying devices is explained in detail in the attached drawings;
(3) the reaction kettle comprises a sol detention area 200, the bottom of the reaction kettle is provided with a discharging bottom valve 100, and the discharging bottom valve 100 is communicated with the sol detention area 200;
(4) the porous screen 300 is arranged in the reaction kettle, a plurality of screen holes 301 are formed in the porous screen 300, and the porous screen 300 is communicated with the sol detention zone 200;
(5) stirring rake 600, electric actuator 500 is connected with stirring rake 600, and electric actuator 500 controls the rotational speed of stirring rake 600.
In one embodiment, the porous screen 300 is the main area for sol preparation, and is a screen with certain aperture diameter woven by stainless steel, and the size of the screen hole 301 can be selected in 100-1000 mesh;
in one embodiment, the aqueous phase of the precipitant 1 and the aqueous phase of the precipitant 2 sprayed by the two spraying devices 400 react to form a solid sol after contacting each other on the porous screen 300, and the solid sol is sieved by the stirring paddle 600; in order to facilitate replacement of the multi-hole screen 300 with different mesh numbers and cleaning, the multi-hole screen 300 designed by the present invention can be freely disassembled.
In one embodiment, the spraying device 400 sprays the precipitant aqueous phase through the spraying holes 402, wherein the size of the spraying holes can be selected and disassembled for replacement, the size and flow rate of the spraying holes can be controlled by the feeding part, and the feeding pipe 403, the spraying head 401 and the spraying holes 402 are connected in sequence to finally form the spraying device 400.
The working principle is as follows: in one embodiment, the electric device 500 is turned on to drive the stirring paddle 600 to rotate, then the precipitant 1 water phase and the precipitant 2 water phase are simultaneously sprayed into the porous screen 300 of the reaction kettle through the spraying device 400, the stirring paddle 600 stirs and disperses the generated solid sol, and simultaneously the newly generated solid sol is transferred to the sol retention zone 200 through the porous screen 300, the sol retention zone 200 is communicated with the discharging bottom valve 100, and after the preparation is finished, the solid sol is discharged through the discharging bottom valve 100.
Example 1
Preparation of magnesium hydroxide solid sol
1kg of 0.15mol/L magnesium nitrate solution and 1kg of 0.6mol/L sodium hydroxide solution are prepared, then under the stirring of the rotating speed of 800rpm, the magnesium nitrate and the sodium hydroxide solution are simultaneously dripped into a porous screen 300 through a spraying device 400, the aperture of the screen is 1000 meshes, and after the dripping is finished, the stirring is continued for 0.5h, thus obtaining the sol-like magnesium hydroxide dispersion liquid.
Example 2
Preparation of aluminum hydroxide solid sol
1kg of 0.2mol/L aluminum nitrate solution and 1kg of 0.75mol/L sodium hydroxide solution are prepared, then aluminum nitrate and sodium hydroxide are simultaneously dripped into a porous screen 300 through a spraying device 400 under the stirring of the rotating speed of 800rpm, the aperture of the screen is 1000 meshes, and after the dripping is finished, the stirring is continued for 0.5h, thus obtaining the sol-like aluminum hydroxide dispersion liquid.
Example 3
Preparation of solid calcium hydroxy phosphate sol
1kg of 1mol/L calcium hydroxide solution is prepared, 1% of sodium dodecyl sulfate needs to be added into the calcium hydroxide solution to assist the calcium hydroxide solution to disperse because the calcium hydroxide is slightly soluble in water, 1kg of 0.5mol/L phosphoric acid solution is prepared, then the calcium hydroxide and the phosphoric acid solution are simultaneously dripped into a porous screen 300 through a spraying device 400 under the stirring of the rotating speed of 1000rpm, the aperture of the screen is 500 meshes, and after the dripping is finished, the stirring is continued for 0.5h, thus obtaining the calcium hydroxy phosphate (HAP) dispersion liquid.
Example 4
Preparation of magnesium carbonate solid sol
1kg of 0.25mol/L sodium carbonate solution and 1kg of 0.25mol/L magnesium sulfate solution are prepared, the magnesium sulfate is dissolved in water, the heat release is obvious, and the magnesium sulfate is required to be gradually added into the water. Then, under the stirring of the rotation speed of 800rpm, the sodium carbonate and magnesium sulfate solution is simultaneously dripped into the porous screen 300 through the spraying device 400, the aperture of the screen is 1000 meshes, after the dripping is finished, the stirring is continued for 0.5h, and the magnesium carbonate dispersion liquid is obtained, and is actually basic magnesium carbonate (Mg (OH)2·MgCO3) Is a double salt of magnesium hydroxide and magnesium carbonate.
Example 5
Taking 1kg of the magnesium hydroxide aqueous phase prepared by the invention as an aqueous phase, uniformly mixing 60g of acrylonitrile, 10g of methyl methacrylate, 30g of methacrylic acid, 0.05g of styrene, 1 part of lauroyl peroxide, 0.5g of divinylbenzene and 0.05g of isopentane to obtain an oil phase, wherein the polymerization temperature is 65 ℃, the polymerization time is 20 hours, and then preparing the expandable microspheres according to the preparation method of the expandable microspheres. The particle diameter of the microsphere is 30um and Ts＝200℃，Tmax＝260℃。
The other preparation methods such as barium sulfate, calcium carbonate, copper oxide and the like can be prepared according to the preparation method of inorganic double decomposition reaction.
The solid sol preparation device and the method of the invention are applied to successfully prepare the expandable microspheres, which shows that the solid sol preparation device and the method of the invention can be used for the production of the expandable microspheres.
Compared with the prior art, the simple device for preparing the solid sol can prepare the uniformly dispersed solid sol by using the porous spray head and the porous screen, solves the problems of complex equipment and small production scale in the preparation of the solid sol, realizes the continuous preparation of the solid sol, can effectively increase the dispersibility of the sol, improves the production efficiency, and simultaneously achieves the purposes of energy conservation and environmental protection.
The invention also provides a method for jointly spraying and dripping, which solves the problem of poor dispersibility in the preparation of the solid sol, can realize the preparation of the solid sol with certain particle size distribution by controlling the aperture size of the porous screen, can successfully use the prepared solid sol for the preparation of the expandable microspheres, improves the reliability and the simplicity of the preparation of the solid sol, effectively improves the operation efficiency, is convenient to process, has low cost and is beneficial to realizing mass production.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A solid sol production apparatus characterized by comprising:
(1) the reaction kettle comprises a sol detention area, the bottom of the reaction kettle is provided with a discharging bottom valve, and the discharging bottom valve is communicated with the sol detention area;
(2) spray assembly sets up at the reation kettle top, includes two or more spray set, spray set includes in proper order on vertical: a feeding pipe, a spray head and spray holes;
(3) the porous screen is arranged in the reaction kettle, is provided with a plurality of screen holes and is communicated with the sol detention zone;
(4) the stirring paddle is arranged in the reaction kettle.
2. The apparatus for preparing a solid sol according to claim 1, wherein the stirring paddle is connected to an electric device for driving the stirring paddle to rotate.
3. The solid sol production apparatus according to claim 1, wherein said spraying means comprises, in order in the longitudinal direction: inlet pipe, shower nozzle, orifice.
4. A method for preparing a solid sol using the apparatus according to any one of claims 1 to 3, comprising the steps of:
s1, feeding: respectively preparing the precipitating agents into water phases, dropwise adding the water phases by the spraying device, forming sol inside the porous screen after the precipitating agents are contacted with each other, and enabling the sol to enter a sol retention area through the porous screen;
s2, dispersing: after the contact of the precipitator, the electric device drives the stirring paddle to carry out shearing dispersion;
s3, discharging: and discharging the solid sol positioned in the sol detention area through the discharging bottom valve.
5. The preparation method according to claim 4, wherein the precipitant comprises precipitant 1 and precipitant 2, and the precipitant 1 is selected from one or more of sodium hydroxide, potassium hydroxide, ammonia water, sodium carbonate and sodium bicarbonate; the precipitant 2 is Mg2+、Al3+、Ca2+、Ba2+、Fe2+、Fe3+One or more soluble salts of metal ions in (a).
6. The preparation method according to claim 5, wherein the content of the precipitant 1 is 5-50 wt% of the aqueous phase; the content of the precipitant 2 is 5-50 wt% of the water phase.
7. The preparation method according to claim 4, wherein a dispersant is further added in the feeding process in step S1, the addition amount of the dispersant is 0.01-5 wt% of the water phase, and the dispersant is selected from one or more of ionic dispersant, nonionic dispersant and polymeric dispersant.
8. The preparation method according to claim 7, wherein the dispersant is an anionic dispersant selected from one or more of sodium oleate, carboxylate, sulfate ester salt and sulfonate.
9. The preparation method according to claim 4, wherein inorganic salt is further added in the feeding process in step S1, the addition amount of the inorganic salt is 0.5-50 wt% of the water phase, and the inorganic salt is selected from one or more of sodium chloride, potassium chloride, magnesium sulfate and aluminum chloride.
10. The method according to claim 4, wherein the discharged solid sol in step S3 has a solid content of 0 to 10%.
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