CN1506305A - Production process of nano rod-like active silica with attapulgite and clay - Google Patents
Production process of nano rod-like active silica with attapulgite and clay Download PDFInfo
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- CN1506305A CN1506305A CNA021485232A CN02148523A CN1506305A CN 1506305 A CN1506305 A CN 1506305A CN A021485232 A CNA021485232 A CN A021485232A CN 02148523 A CN02148523 A CN 02148523A CN 1506305 A CN1506305 A CN 1506305A
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Abstract
The production process of nano rod-like active silica is one acid dissolving process with attapulgite and clay as material. The positive effects of the present invention include elimination of high temperature alkali dissolving process, reduced material consumption and lowered production cost. Compared with traditional technological process, the nano rod-like active silica product of the present invention has ever high physical and chemical characteristics, including original concentration, dispersive performance and shape features. The present invention has wide application value.
Description
Technical field:
The present invention relates to nonmetal mineral resource deep processing and technical field of inorganic chemical industry.More specifically say so and produce the method for nano bar-shape active silica with attapulgite clay.
Background technology:
Active silica (white carbon black) is the unformed fine powder of white, light weight, proportion 2.319-2.653,1750 ℃ of fusing points.Very high insulativity is arranged, water insoluble and sour, be dissolved in caustic soda and hydrofluoric acid.Active silica is used as natural rubber and elastomeric reinforcing filler, also can make soft rumbling compound, the paint matting agent of filler for plastic, lubricant, insulating material, coating anti-settling agent, synthetic resins weighting agent, printing ink thickening material, vehicle and metal.Active silica is a kind of widely used inorganic chemical industry material.At present, conventional preparation method is by siliceous material, as high temperature alkali fusions such as quartz sand, opals, and the water-soluble liquid soluble glass that becomes, sour again wash rice dehydrates and makes.This complex technical process, consuming a large amount of soda ash and acid is the high root of its cost.
Summary of the invention:
Technical problem to be solved by this invention is to avoid existing problem in the above-mentioned prior art, provide that a kind of raw materials consumption is few, technology is simple, production cost is low, and can make product have the method for producing the nano bar-shape active silica with attapulgite clay of more excellent physicochemical property.
The technical scheme that technical solution problem of the present invention is adopted is:
Technical characterstic of the present invention is to be raw material with the attapulgite clay, makes silicon-dioxide with acid pasting.
By from nanoscale to the intensive research of the molten effect of attapulgite acid, find that attapulgite forms nano bar-shape active silica (white carbon black) in the sour molten process that is fit to.The present invention utilizes the technology of the molten production active silica of attapulgite acid to be acid-soluble one-step.Compared with the prior art, beneficial effect of the present invention is embodied in the high temperature alkali fuse process of having save, and raw material consumption reduces, and production cost reduces.Nano bar-shape active silica original particle size, the dispersing property of producing with the inventive method, morphological specificity is compared with spherical active three silicon oxide of traditional technology preparation that more excellent physicochemical property is arranged, and has potential widely using value.
Fig. 1 is the transmission electron microscope image, shows nano bar-shape active silica (white carbon black) form with the inventive method preparation.
Fig. 2 is an X-luminous energy spectrogram, shows nano bar-shape active silica (white carbon black) composition with the inventive method preparation.
Fig. 3 is technological process of production figure of the present invention.
Embodiment:
Present embodiment is to be raw material with the attapulgite clay, and a step direct acid-soluble method is produced the nano bar-shape active silica.
Fig. 1 and Fig. 2 show the form and the composition of nano bar-shape active silica respectively.Its ultimate principle is that octahedral cations Mg, Al in the attapulgite structure, Fe can dissolve under the strong acid effect fully, and as attapulgite silica backbone's SiO
2Keep the crystal habit of attapulgite, thereby produce nano bar-shape active silica (white carbon black).
The concrete enforcement of present embodiment is not less than 60% with the attapulgite content in the attapulgite clay, and mineral such as quartz, feldspar are not higher than 5% and are advisable.Quartzy, feldspar content is few more good more, the few more acid consumption that can reduce chemical reaction of rhombspar content.
The used acid of acid pasting comprises hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid or mixing acid in the present embodiment.Chemical reaction temperature can be controlled at 50-130 ℃, and temperature is high more, and the time of reaction needed is short more.Chemical reaction can be finished under normal pressure, also can finish in autoclave pressure, and pressure is at 1-10 normal atmosphere.Comparatively high temps and pressure can improve speed of response in the autoclave pressure.
Referring to Fig. 3, concrete production process and main technical details are as follows:
1, suitable ore type is selected in attapulgite clay ore bed layer mining, and the content of general requirement attapulgite is not less than 60%, and quartzy and feldspar content is not higher than 5%.Quartzy and feldspar all is mineral, and for being the raw material production active silica with the attapulgite clay, they all are impurity and objectionable constituent.
2, carry out drying treatment when water content is too high, the concrete industrial scale weather condition of dry basis can be considered natural air drying or drying machine drying, and the general requirement water content is less than 20%.
3, satisfy under the prerequisite of pulverizing requirement in water content, carry out comminution process, grinding particle size requires 100% to cross 100 orders.
4, sour molten reaction is the key point in this enforcement, uses inorganic acid or mixing acid such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, and acid concentration is 5-50%, and optimum concn is 25%.Temperature of reaction 50-130 ℃, reaction pressure is at 1-10 normal atmosphere, and the reaction times is specifically controlled according to the different of reaction conditions, after 1000 ℃ of calcinations of solids, and MgO+Al
2O
3+ Fe
2O
3Content is less than 3%, SiO
2Greater than 95%.
5, the molten reaction of acid back is carried out solid-liquid separation and is carried out washing operation by solid-liquid separating equipment.Specifically can be in dehydration equipment, to carry out backwash, have backwash system and operation as some plate-and-frame filter press.
6, solid product obtains product by drying, dispersion and packing.
Claims (6)
1, a kind of method of producing the nano bar-shape active silica with attapulgite clay is characterized in that with the attapulgite clay being raw material, makes silicon-dioxide with acid pasting.
2, method of producing the nano bar-shape active silica with attapulgite clay according to claim 1 is characterized in that concrete steps are:
The ore type that is fit to is selected in a, the layer mining of attapulgite clay ore bed;
B, when water content is too high, carry out drying treatment;
C, under the prerequisite that water content satisfy to pulverize requires, pulverize;
D, sour molten reaction, after the solids calcination, MgO+AL
2O
3+ Fe
2O
3Content is less than 3%, SiO
2Greater than 95%;
E, solid-liquid separation, washing;
F, solid product drying, dispersion and packing are gained.
3, method of producing the nano bar-shape active silica with attapulgite clay according to claim 1 and 2 is characterized in that attapulgite content is not less than 60% in described attapulgite clay as raw material, and mineral such as quartz, feldspar are not higher than 5%.
4,, it is characterized in that described attapulgite clay water content as raw material is less than 20% according to claim 1 or 2 described methods of producing the nano bar-shape active silica with attapulgite clay.
5, method of producing the nano bar-shape active silica with attapulgite clay according to claim 1 and 2 is characterized in that the used acid of described acid pasting comprises hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid or mixing acid.
6, method of producing the nano bar-shape active silica according to claim 1 and 2 with attapulgite clay, the acid concentration that it is characterized in that described acid solution is 5-50%, and temperature of reaction is 50-130 ℃, and reaction pressure is at 1-10 normal atmosphere.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021485232A CN1219698C (en) | 2002-12-10 | 2002-12-10 | Production process of nano rod-like active silica with attapulgite and clay |
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| CNB021485232A CN1219698C (en) | 2002-12-10 | 2002-12-10 | Production process of nano rod-like active silica with attapulgite and clay |
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| CN1506305A true CN1506305A (en) | 2004-06-23 |
| CN1219698C CN1219698C (en) | 2005-09-21 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329337C (en) * | 2005-02-28 | 2007-08-01 | 江苏南大紫金科技集团有限公司 | Preparation method of one-dimensional nano silicate clay |
| CN100355694C (en) * | 2006-03-14 | 2007-12-19 | 合肥工业大学 | Magnetic particle-attapulgite composite nano material and preparation method by directly dissolving attapulgite in acid |
| CN100377997C (en) * | 2006-05-21 | 2008-04-02 | 戴福寿 | Method for extracting nano silicon dioxide from calcium-base bentonite |
| CN101434393B (en) * | 2007-11-16 | 2010-11-10 | 辽宁科技大学 | Method for preparing nano-scale amorphous silica from attapulgite clay |
| CN101367960B (en) * | 2008-09-12 | 2010-12-29 | 江苏工业学院 | Preparation method for composite material of nano-concave-convex stick stone/silicon dioxide |
| CN102284279A (en) * | 2010-06-18 | 2011-12-21 | 中国石油化工股份有限公司 | Attapulgite/silicon dioxide composite powder and preparation method thereof |
| CN102491351A (en) * | 2011-12-13 | 2012-06-13 | 沈阳化工大学 | Method for preparing white carbon black through natural clinoptilolite |
| CN104577082A (en) * | 2015-01-09 | 2015-04-29 | 南京大学 | Nano-silicon material and application thereof |
| CN107804854A (en) * | 2017-11-27 | 2018-03-16 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | The method that cupric silicate nanotube is prepared using low-grade attapulgite clay |
| CN110436471A (en) * | 2019-09-06 | 2019-11-12 | 中国科学院兰州化学物理研究所 | The method for preparing the mixed dimension nano silicon material of white using red attapulgite stone clay |
-
2002
- 2002-12-10 CN CNB021485232A patent/CN1219698C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329337C (en) * | 2005-02-28 | 2007-08-01 | 江苏南大紫金科技集团有限公司 | Preparation method of one-dimensional nano silicate clay |
| CN100355694C (en) * | 2006-03-14 | 2007-12-19 | 合肥工业大学 | Magnetic particle-attapulgite composite nano material and preparation method by directly dissolving attapulgite in acid |
| CN100377997C (en) * | 2006-05-21 | 2008-04-02 | 戴福寿 | Method for extracting nano silicon dioxide from calcium-base bentonite |
| CN101434393B (en) * | 2007-11-16 | 2010-11-10 | 辽宁科技大学 | Method for preparing nano-scale amorphous silica from attapulgite clay |
| CN101367960B (en) * | 2008-09-12 | 2010-12-29 | 江苏工业学院 | Preparation method for composite material of nano-concave-convex stick stone/silicon dioxide |
| CN102284279B (en) * | 2010-06-18 | 2013-02-27 | 中国石油化工股份有限公司 | Attapulgite/silicon dioxide composite powder and preparation method thereof |
| CN102284279A (en) * | 2010-06-18 | 2011-12-21 | 中国石油化工股份有限公司 | Attapulgite/silicon dioxide composite powder and preparation method thereof |
| CN102491351A (en) * | 2011-12-13 | 2012-06-13 | 沈阳化工大学 | Method for preparing white carbon black through natural clinoptilolite |
| CN104577082A (en) * | 2015-01-09 | 2015-04-29 | 南京大学 | Nano-silicon material and application thereof |
| CN107804854A (en) * | 2017-11-27 | 2018-03-16 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | The method that cupric silicate nanotube is prepared using low-grade attapulgite clay |
| CN107804854B (en) * | 2017-11-27 | 2020-03-17 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Method for preparing copper silicate nanotube by using low-grade attapulgite clay |
| CN110436471A (en) * | 2019-09-06 | 2019-11-12 | 中国科学院兰州化学物理研究所 | The method for preparing the mixed dimension nano silicon material of white using red attapulgite stone clay |
| CN110436471B (en) * | 2019-09-06 | 2022-10-28 | 中国科学院兰州化学物理研究所 | Method for preparing white dimension-mixed nano silicon material by using red attapulgite clay |
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| Publication number | Publication date |
|---|---|
| CN1219698C (en) | 2005-09-21 |
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