CN114538456A - Preparation method of high-whiteness attapulgite-based inorganic gel - Google Patents
Preparation method of high-whiteness attapulgite-based inorganic gel Download PDFInfo
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- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 73
- 229960000892 attapulgite Drugs 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000725 suspension Substances 0.000 claims abstract description 62
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000010494 dissociation reaction Methods 0.000 claims abstract description 15
- 230000005593 dissociations Effects 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 10
- 150000003608 titanium Chemical class 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000004537 pulping Methods 0.000 claims abstract description 5
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 20
- 239000013078 crystal Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000012065 filter cake Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 6
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 4
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- 239000006004 Quartz sand Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 229960003339 sodium phosphate Drugs 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 2
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 2
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 239000002537 cosmetic Substances 0.000 abstract description 6
- 239000003973 paint Substances 0.000 abstract description 6
- 230000002087 whitening effect Effects 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 239000002562 thickening agent Substances 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract description 2
- 229910017053 inorganic salt Inorganic materials 0.000 abstract 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 21
- 239000000843 powder Substances 0.000 description 18
- 239000007787 solid Substances 0.000 description 11
- 229910052500 inorganic mineral Inorganic materials 0.000 description 8
- 239000011707 mineral Substances 0.000 description 8
- 235000010755 mineral Nutrition 0.000 description 8
- 238000004062 sedimentation Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 239000000084 colloidal system Substances 0.000 description 4
- 238000009775 high-speed stirring Methods 0.000 description 4
- 238000011085 pressure filtration Methods 0.000 description 4
- 230000001360 synchronised effect Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002734 clay mineral Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000000606 toothpaste Substances 0.000 description 2
- 229940034610 toothpaste Drugs 0.000 description 2
- QILJBEAPSAEXMR-UHFFFAOYSA-L [Mg+2].[Cl-].OP(O)([O-])=O Chemical compound [Mg+2].[Cl-].OP(O)([O-])=O QILJBEAPSAEXMR-UHFFFAOYSA-L 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- XONPDZSGENTBNJ-UHFFFAOYSA-N molecular hydrogen;sodium Chemical compound [Na].[H][H] XONPDZSGENTBNJ-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/62—L* (lightness axis)
Abstract
The invention discloses a preparation method of high-whiteness attapulgite-based inorganic gel, which comprises the steps of sequentially crushing, three-roll extruding, pulping, activating and cyclone grading natural attapulgite raw ore to obtain purified suspension, and adding inorganic salt into the purified suspension for ultrasonic treatment to obtain dissociation modified suspension; then the high-whiteness attapulgite-based inorganic gel is obtained after titanium salt or titanium oxide modification, solid-liquid separation and drying treatment. The invention prepares the high-whiteness attapulgite by purifying, synchronously dissociating, tackifying and whitening and modifying the natural attapulgiteL*Value up to 85), excellent suspension stability and high viscosity (initial viscosity)>2000 mpa.s) can be used as a suspension stabilizer or a thickening agent to be applied to the fields of high-end paint, cosmetics, biomedicine and the like.
Description
Technical Field
The invention relates to a preparation method of a mineral inorganic gel, in particular to a preparation method of a high-whiteness attapulgite-based inorganic gel, belonging to the technical field of nano mineral functional material preparation and nonmetal ore deep processing.
Background
In the industries of high-end coating, textile, paper making, daily chemicals (such as cosmetics, toothpaste and facial cleanser) and the like, a large amount of gel auxiliaries such as thickening agents, adhesives, thixotropic agents and the like are required to be used. In recent years, the technology and process for preparing inorganic gel by using natural clay mineral are receiving extensive attention, and some representative industrial products are formed primarily, for example, bentonite thickening rheological agent is applied in the fields of daily chemicals and coatings. Therefore, the inorganic gel prepared by utilizing natural clay minerals which are abundant in reserves and come from nature has huge market potential and comprehensive competitiveness. With the rapid development of high-end product industry and the continuous upgrading and updating of products, the dosage of the tackifier and the thickener is gradually increased year by year, the requirements on suspension stability, viscosity, thixotropy, electrolyte resistance and the like are increasingly improved, and the requirements on whiteness in the fields of cosmetics, toothpaste, paint and the like are increasingly high. Therefore, there is an urgent need to develop a high whiteness mineral inorganic gel to meet the market demand and industry development of high-end products.
As is well known, attapulgite is a clay mineral with one-dimensional nano rod-shaped crystal morphology, adjustable surface charge and excellent colloid performance, can thicken various systems such as a pure water system, an electrolyte and the like, and is one of ideal materials for preparing mineral gel. For example, Chinese invention patents CN107555445B 'an inorganic gel of magnesium aluminum silicate and a preparation method thereof', CN107902662A 'a preparation method of inorganic gel of magnesium aluminum silicate with high dispersibility and high viscosity', CN110734073A 'a preparation method of inorganic gel with double network structure assembled by gel factor attapulgite', CN102476805B 'a method for improving colloid stability of attapulgite clay', CN103395797B 'a method for improving colloid performance of attapulgite clay by using bischofite', and the like relate to a preparation method and application of attapulgite-based mineral gel. In addition, the upgrading and upgrading of high-end cosmetics, paints, pigments and the like are closely related to the development of whitening technology. The Chinese invention patents CN111936109A ' white pigment for cosmetics, CN103140556B ' water-based paint composition ', CN104774538B ' high-gloss high-whiteness heat-dissipation insulating paint and a preparation method thereof ', CN105092571B ' a rapid detection method for application performance of titanium dioxide in an oil paint system ' and CN10649714B ' a preparation method for titanium dioxide pigment with high covering power, high weather resistance and high whiteness ' relate to the improvement of physical and chemical properties of whiteness and the like of products by using titanium salt. According to the invention, the mineral inorganic gel with high whiteness, good suspension stability and good dispersibility is prepared by performing combined processes such as purification, synchronous dissociation and adhesion promotion, modification treatment and the like on the natural attapulgite raw ore, and the technology or the process has no related research report and no application precedent.
Disclosure of Invention
The invention aims to overcome the defects of non-ideal suspension stability, low whiteness and the like of mineral inorganic gel, and provides a preparation method of high-whiteness attapulgite-based inorganic gel by means of attapulgite rod crystal beam dissociation and the like on the basis of fully knowing the crystal structure and physicochemical characteristics of attapulgite. The dispersion degree, surface charge and suspension stability of attapulgite rod crystals are changed by activating, purifying, synchronously dissociating and tackifying natural attapulgite raw ores, and a mineral inorganic gel with high whiteness is further prepared efficiently by modification treatment and whitening and can be used as a whitening agent, a suspension stabilizer, a thickening agent or a rheological aid for high-end coatings, cosmetics, biomedicine or daily chemicals and the like.
The invention relates to a preparation method of high-whiteness attapulgite-based inorganic gel, which comprises the steps of crushing and three-roll extrusion treatment of natural attapulgite raw ore (the distance between two adjacent rolls is kept between 0.3 and 0.6mm, the attapulgite raw ore is used for bulking and tearing attapulgite rod crystal bundles or aggregates and is beneficial to hydration expansion and depolymerization dispersion), dispersing the attapulgite raw ore into an acidic aqueous solution for pulping and activation for 4 to 6 hours, and removing insoluble large granular substances such as quartz sand and the like through cyclone classification treatment to obtain purified suspension; adding a modifier into the purified suspension for ultrasonic dissociation and synchronous modification to obtain attapulgite rod crystal beam dissociation modified suspension; and then adding titanium salt or titanium dioxide into the attapulgite rod crystal bundle dissociation modified suspension, adjusting the pH value to 8-10, stirring at room temperature for 2-8 h, carrying out filter pressing to obtain a filter cake with the water content of 40-50%, carrying out roller extrusion on the filter cake to obtain a sheet with the thickness of 1-2 mm, and carrying out strong drying treatment to obtain the high-whiteness attapulgite-based inorganic gel.
The content of attapulgite in the natural attapulgite raw ore is not less than 50 percent. The solid-to-liquid ratio of the natural attapulgite raw ore in the acidic aqueous solution is 50-100 kg/m3。
The acidic aqueous solution is one of sulfuric acid, hydrochloric acid or phosphoric acid aqueous solutions, and the pH value of the solution is 3.5-5.0.
The content of quartz sand in the purification suspension is not higher than 1%.
The modifier is at least one of sodium hexametaphosphate, sodium pyrophosphate, sodium phosphate, sodium dihydrogen phosphate, sodium tripolyphosphate, sodium polyphosphate, ammonium sulfate, ammonium bisulfate, ammonium chloride, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium carbonate, sodium carbonate, ammonium carbonate, magnesium nitrate, magnesium hydroxide, magnesium sulfate, magnesium chloride and magnesium oxide. The addition amount of the modifier is 0.25-5.0% of the mass of the natural attapulgite raw ore.
The ultrasonic treatment is carried out at an ultrasonic power of 60-200 KHZ and for a treatment time of 5-15 min.
The titanium salt is any one of titanium sulfate and titanyl sulfate. The addition amount of the titanium salt or the titanium dioxide is 10 to 20 percent of the mass of the natural attapulgite raw ore.
The pH value is adjusted by adopting 4mol/L sodium hydroxide solution.
CIE-L*a*b*The color parameters are shown in table 1. As can be seen from Table 1, the method for preparing the attapulgite inorganic gel productL*The value is as high as 85.12, and the whiteness is (relative to the attapulgite raw ore) ((L*A value of 68.57) is greatly improved. The color difference between the gel product and the raw ore after pulping is shown in figure 1. As can be seen from the digital pictures, the raw ore suspension (solid content of 7%) contains black particles and gravel, is yellowish brown in appearance, and has a high speed of 11000rpmStirring for 20min, standing for 72h, and settling rate is 6%; the attapulgite inorganic gel product suspension prepared by the invention is stable, uniform and white, and the obtained suspension is stirred at high speed under the same condition and then stands for 72 hours, the sedimentation rate is less than or equal to 2 percent, and the stable suspension and the colloidal property are shown. FIG. 2 is a rotational viscosity change curve of the attapulgite inorganic gel prepared by the invention, wherein the rotational viscosity determination method is as follows: 28g of the sample was dispersed in 372mL of water, and after stirring at 11000rpm for 20min at high speed, the viscosity value was measured with an NDJ-8S rotary viscometer, and a No. 3 rotor was selected at 30 rpm. According to the viscosity data, the initial rotary viscosity of the attapulgite raw ore is 1468mPa.s, and the rotary viscosity is reduced to 844mPa.s with the extension of the shearing time to 10min, but the initial rotary viscosity of the attapulgite inorganic gel product prepared by the method can reach 2017mPa.s to the maximum, and the rotary viscosity value is still 1236mPa.s after the attapulgite inorganic gel product is sheared for 10min, which indicates that the suspension system has higher viscosity and good colloid performance.
In conclusion, the attapulgite-based inorganic gel product with high whiteness and excellent colloidal property and dispersibility is obtained through various processes such as acid activation, cyclone purification, synchronous rod crystal beam dissociation and tackifying and the like, the dispersity, the purity and the surface charge of the attapulgite are changed, the colloidal properties such as the viscosity, the suspension stability and the like of the attapulgite are improved, and the attapulgite-based inorganic gel product is further subjected to whitening treatment. In addition, the invention fully utilizes the cavitation of ultrasonic treatment and the acceleration effect on chemical reaction, is beneficial to the high-efficiency dissociation and synchronous tackifying of the attapulgite rod crystal beam, has green and high-efficiency whole preparation process, does not involve the use of high-temperature and high-pressure equipment, can recycle the liquid after solid-liquid separation, is easy to control the preparation process, and is beneficial to realizing industrial batch production.
Drawings
FIG. 1 is a digital picture of a suspension after pulping of the attapulgite-based inorganic gel product prepared by the present invention;
FIG. 2 is a rotational viscosity change curve of the attapulgite-based inorganic gel product prepared according to the present invention.
Detailed Description
The preparation method and the product of the high-whiteness attapulgite inorganic gel of the invention are further explained by the specific examples below.
Example 1
Crushing 200kg of natural attapulgite raw ore, extruding with three rollers (the distance between two adjacent rollers is kept at 0.6 mm), and uniformly dispersing to 3m3Mechanically stirring and reacting for 4h in sulfuric acid aqueous solution (pH = 3.5), and then carrying out three-stage cyclone classification treatment on the suspension to obtain purified suspension; and adding 0.5kg of solid sodium dihydrogen magnesium chloride phosphate powder into the purified suspension, carrying out ultrasonic treatment for 5min at the power of 60KHZ, adding 20kg of solid titanium oxysulfate powder into the obtained rod-crystal beam dissociation modified suspension, adjusting the pH to be =8 by using 4mol/L sodium hydroxide solution, stirring at room temperature for reaction for 4h, carrying out filter pressing to obtain a filter cake, carrying out roller extrusion to obtain a 1mm sheet, and carrying out forced drying treatment (the drying temperature is 90 ℃) to obtain a powder product, wherein the powder product is marked as APT-Gel-1. 7g of APT-Gel-1 sample is taken to be dispersed in 93mL of water, the suspension is prepared after high-speed stirring is carried out for 20min at 11000rpm, the suspension is filled into a 100mL measuring cylinder, and the sedimentation rate is measured to be about 2% after the suspension is kept stand for 72 h. CIE of APT-Gel-1L*a*b*The color parameters are shown in table 1.
Example 2
Crushing 200kg of natural attapulgite raw ore, performing three-roller extrusion treatment (the distance between two adjacent rollers is kept at 0.6 mm), and uniformly dispersing to 3m3Mechanically stirring in hydrochloric acid aqueous solution (pH = 3.5) for reacting for 4h, and performing three-stage cyclone classification treatment on the suspension to obtain purified suspension; and adding 1kg of sodium dihydrogen phosphate solid powder into the purified suspension, carrying out ultrasonic treatment for 10min at the power of 80KHZ, adding 20kg of titanium dioxide solid powder into the obtained rod-crystal beam dissociation modified suspension, adjusting the pH to be =9 by adopting 4mol/L sodium hydroxide solution, stirring for reaction for 4h, carrying out pressure filtration to obtain a filter cake, extruding the filter cake into a 1mm thin sheet by using a roller, and carrying out forced drying treatment (the drying temperature is 100 ℃, and the grading frequency is 8 HZ) to obtain a powder product, wherein the powder product is marked as APT-Gel-2. Dispersing 7g of APT-Gel-2 sample in 93mL of water, stirring at 11000rpm for 20min to obtain suspension, and filling 100mL of the suspensionIn the measuring cylinder, the sedimentation rate after standing for 72 hours is measured to be about 2%. CIE of APT-Gel-2L*a*b*The color parameters are shown in table 1.
Example 3
Crushing 200kg of natural attapulgite raw ore, extruding with three rollers (the distance between two adjacent rollers is kept at 0.3 mm), and uniformly dispersing to 3m3Mechanically stirring and reacting in sulfuric acid aqueous solution (pH = 4) for 6h, and then carrying out three-stage cyclone classification treatment on the suspension to obtain purified suspension; and adding 1kg of magnesium chloride and 2kg of disodium hydrogen phosphate solid powder into the purified suspension, carrying out ultrasonic treatment for 10min at the power of 100KHZ, adding 30kg of titanyl sulfate solid powder into the obtained rod-crystal beam dissociation modified suspension, adjusting the pH to be =10 by using 4mol/L sodium hydroxide solution, stirring for reacting for 6h, carrying out pressure filtration to obtain a filter cake, extruding the filter cake into a 1mm sheet by using a roller, and carrying out forced drying treatment (the drying temperature is 110 ℃, the grading frequency is 25 HZ) to obtain a powder product which is marked as APT-Gel-3. 7g of APT-Gel-3 sample is taken to be dispersed in 93mL of water, the suspension is prepared after high-speed stirring is carried out for 20min at 11000rpm, the suspension is filled into a 100mL measuring cylinder, and the sedimentation rate is measured to be about 1.5% after the suspension is kept stand for 72 h. CIE of APT-Gel-3L*a*b*The color parameters are shown in table 1.
Example 4
Crushing 200kg of natural attapulgite raw ore, extruding with three rollers (the distance between two adjacent rollers is kept at 0.5 mm), and uniformly dispersing to 3m3Mechanically stirring and reacting for 6 hours in phosphoric acid aqueous solution (pH = 5), and then carrying out three-stage cyclone classification treatment on the suspension to obtain purified suspension; and adding 2kg of magnesium oxide and 2kg of sodium dihydrogen phosphate solid powder into the purified suspension, carrying out ultrasonic treatment for 15min at the power of 150KHZ, adding 40kg of titanyl sulfate solid powder into the obtained rod-crystal beam dissociation modified suspension, adjusting the pH to be =10 by adopting 4mol/L sodium hydroxide solution, stirring for reacting for 6h, carrying out pressure filtration to obtain a filter cake, extruding the filter cake into a 1mm sheet by a pair of rollers, and carrying out forced drying treatment (the drying temperature is 100 ℃, and the grading frequency is 8 HZ) to obtain a powder product which is marked as APT-Gel-4. 7g of APT-Gel-4 sample is taken to be dispersed in 93mL of water, the suspension is prepared after high-speed stirring is carried out for 20min at 11000rpm, the suspension is filled into a 100mL measuring cylinder, and the sedimentation rate is measured to be about 1% after the suspension is kept stand for 72 h. CIE of APT-Gel-4-L*a*b*Color parameters are shown in the table1。
Example 5
Crushing and extruding 200kg natural attapulgite raw ore (the distance between two adjacent rollers is kept at 0.4 mm), and uniformly dispersing to 3m3Mechanically stirring and reacting for 4h in sulfuric acid aqueous solution (pH = 4.5), and then carrying out three-stage cyclone classification treatment on the suspension to obtain purified suspension; and adding 2kg of magnesium sulfate and 8kg of ammonium dihydrogen phosphate solid powder into the purified suspension, carrying out ultrasonic treatment for 5min under the power of 200KHZ, adding 30kg of titanium dioxide solid powder into the obtained rod-crystal beam dissociation modified suspension, adjusting the pH to be =10 by adopting 4mol/L sodium hydroxide solution, stirring for reacting for 6h, carrying out pressure filtration to obtain a filter cake, carrying out roller extrusion to obtain a 1mm thin sheet, and carrying out forced drying treatment (the drying temperature is 100 ℃, the grading frequency is 25 HZ) to obtain a powder product, wherein the powder product is marked as APT-Gel-5. 7g of APT-Gel-5 sample is taken to be dispersed in 93mL of water, the suspension is prepared after high-speed stirring is carried out for 20min at 11000rpm, the suspension is filled into a 100mL measuring cylinder, and the sedimentation rate is measured to be about 2% after the suspension is kept stand for 72 h. CIE of APT-Gel-5L*a*b*The color parameters are shown in table 1.
Comparative example
Taking 7g of attapulgite raw ore (marked as APT) sample, dispersing in 93mL of water, stirring at 11000rpm for 20min to prepare a suspension, then filling the suspension into a 100mL measuring cylinder, and standing for 72h to test that the sedimentation rate is about 6%.
Claims (10)
1. A preparation method of high-whiteness attapulgite-based inorganic gel comprises the steps of crushing and three-roll extrusion treatment of natural attapulgite raw ore, dispersing the crushed natural attapulgite raw ore into an acidic aqueous solution, pulping and activating for 4-6 hours, and carrying out cyclone classification treatment to obtain a purified suspension; adding a modifier into the purified suspension for ultrasonic treatment to obtain modified suspension for dissociation of attapulgite rod crystal beams; and then adding titanium salt or titanium dioxide into the attapulgite rod crystal bundle dissociation modified suspension, adjusting the pH value to 8-10, stirring at room temperature for 2-8 h, carrying out filter pressing to obtain a filter cake with the water content of 40-50%, carrying out roller extrusion on the filter cake to obtain a sheet with the thickness of 1-2 mm, and carrying out strong drying treatment to obtain the high-whiteness attapulgite-based inorganic gel.
2. The method for preparing the high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the method comprises the following steps: the content of attapulgite in the natural attapulgite raw ore is not lower than 50 percent; the solid-to-liquid ratio of the natural attapulgite raw ore in the acidic aqueous solution is 50-100 kg/m3。
3. The method for preparing the high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the method comprises the following steps: the acidic aqueous solution is one of sulfuric acid, hydrochloric acid or phosphoric acid aqueous solution, and the pH value of the acidic aqueous solution is 3.5-5.0.
4. The method for preparing the high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the method comprises the following steps: the content of quartz sand in the purification suspension is not higher than 1%.
5. The method for preparing the high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the method comprises the following steps: the modifier is at least one of sodium hexametaphosphate, sodium pyrophosphate, sodium phosphate, sodium dihydrogen phosphate, sodium tripolyphosphate, sodium polyphosphate, ammonium sulfate, ammonium bisulfate, ammonium chloride, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium carbonate, sodium carbonate, ammonium carbonate, magnesium nitrate, magnesium hydroxide, magnesium sulfate, magnesium chloride and magnesium oxide.
6. The preparation method of the high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the addition amount of the modifier is 0.25-5.0% of the mass of the raw ore of the natural attapulgite.
7. The method for preparing the high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the method comprises the following steps: the ultrasonic treatment is carried out at an ultrasonic power of 60-200 KHZ and for a treatment time of 5-15 min.
8. The method for preparing high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the titanium salt is any one of titanium sulfate and titanyl sulfate.
9. The preparation method of the high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the addition amount of the titanium salt or the titanium dioxide is 10-20% of the mass of the natural attapulgite raw ore.
10. The method for preparing the high-whiteness attapulgite-based inorganic gel according to claim 1, wherein the pH value is adjusted by using 4mol/L sodium hydroxide solution.
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