CN1102126C - Calcining and converting reaction process of preparing white carbon with clay mineral - Google Patents

Calcining and converting reaction process of preparing white carbon with clay mineral Download PDF

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CN1102126C
CN1102126C CN98112175A CN98112175A CN1102126C CN 1102126 C CN1102126 C CN 1102126C CN 98112175 A CN98112175 A CN 98112175A CN 98112175 A CN98112175 A CN 98112175A CN 1102126 C CN1102126 C CN 1102126C
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white carbon
carbon black
clay mineral
calcining
kaolin
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CN1244496A (en
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张其春
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Abstract

The present invention relates to calcination conversion reaction technology for preparing white carbon black by using clay minerals. The present invention has the aim of solving problems of poor whiteness and amorphous property of the white carbon black directly prepared by using the clay minerals without passing through a water glass state. The method comprises the technology steps: compounding the clay minerals and solid reactant in the weight ratio of 1 to 3-5 so as to carry out pulverization to less than 100 meshes of granularity, and carrying out calcination for more than 0.5 hour at 360 to 750 DEG C; 2) dissolving calcination production by adding water; 3) carrying out filtration so as to obtain salt containing aluminium from filter liquor, and washing and drying filter cakes so as to obtain the white carbon black, namely amorphous silicon dioxide. X-ray diffraction patterns of the amorphous silicon dioxide present amorphous characteristics, and R457 whiteness reaches 95%.

Description

Calcining and converting reaction process with preparing white carbon with clay mineral
The present invention relates to the manufacture method of white carbon black, particularly via the technology of calcining and converting reaction with preparing white carbon with clay mineral.
The existing method for preparing white carbon black from kaolin comprises two big classes: the first kind is that kaolin is carried out acid is molten, lixiviate goes out aluminium matter component, with siliceous solid formation and the alkali reaction that stays, be converted into sodium silicate solution (water glass), wet method Preparation of White Carbon Black method routinely is settled out white carbon black from sodium silicate solution then; Second class is that kaolinic most aluminium matter components are gone out through repeating sour molten lixiviate, the more siliceous thing of the solid phase in the suspension is separated from aluminum salt solution, directly with as white carbon black.Above-mentioned two class methods all belong to the liquid-solid phase reaction.
H.C.Park et.al. is at Preparation of Alumina and Amorphous Silica fromClay Minerals.J.of the Korean Ceramic Society, 26 (1): the method for the H.C.Pack et.al that is recorded and narrated in 81,1989 can be used as the representative of above-mentioned first kind method.They are raw material with the calcined kaolin, from calcined kaolin, heat acidleach with sulphuric acid soln and go out aluminium matter component, separate through solid-liquid, by reclaiming aluminium in the filtrate, institute obtains siliceous filter cake, and pressurization transforms (NaOH solution was through reaction in 200 ℃, 3 hours) or dry method (reagent is solid Na through wet method 2CO 3, through 1400 ℃ of calcination reactions, calcinate aquation 3 hours in 150 ℃ of autoclave pressures), be converted into sodium silicate solution.Use 5%H 2SO 4With the effect of obtaining sodium silicate solution, therefrom be settled out amorphousness SiO 2, i.e. white carbon black.
Whether through calcining in advance, the above-mentioned second class preparation method can be divided into two subclass again by used kaolin raw material.The kaolin raw material process precalcining that first subclass is used, as Zhang Xingfa in " kaolin system aluminium chlorohydroxide and white carbon black " " chemical engineer " (5): 22,1994 and " producing the experimental study of white carbon black with kaolin " " Anhui chemical industry " (4): 30, in 1,994 two documents, Huang Xiaomin is in " utilizing kaolinite (or kaolin) to produce the research of polymerize aluminum chloride and white carbon black " " nonmetalliferous ore " (2): 30, record and narrate in 1991, adopting 600 ℃ or 750 ℃ of precalcinings, is γ-Al with the alumina octahedral lamella that transforms in the kaolin crystalline structure 2O 3(γ-the Al that is generated 2O 3Be soluble in acid, its sour molten reactive behavior more not interior alumina octahedral lamella of calcined kaolin greatly improves), then through two sections heating acidleach or three sections heating acidleach, the γ-Al in the calcined kaolin 2O 3And Fe 2O 3Be dissolved in the acid Deng material, and the siliceous component in the calcined kaolin is insoluble to acid, is suspended in the acid solution with the silicon powder form, after solid-liquid separates, washs, dries, is the white carbon black product.The used kaolin of second subclass is without precalcining, as Li Yizhi etc. in " kaolin prepares method for white carbon black research " " chemistry world " (5): 198, record and narrate in 1988, directly through first sulfuric acid, back two sections of hydrochloric acid heating acidleach from the kaolin lattice with the stripping by force of lattice aluminium, after solid-liquid separates, the SiO in the former kaolinite 2Remaining in the filter cake, is the white carbon black product after drying, and Chinese patent CN1046507A " kaolin is produced the method for poly aluminium chloride and white carbon black " and the method for being recorded and narrated in above-mentioned " kaolin prepares method for white carbon black research " are similar.
The above-mentioned second class preparation method can not remove and cause colored foreign TiO in the kaolin 2(mainly existing with anatase form, is rutile secondly), the molten back of acid TiO 2To enter in the white carbon black product, work as TiO 2Original content when higher, can significantly reduce the whiteness and the amorphousness characteristic thereof of the white carbon black product that obtains.In addition, the used kaolin raw material of second subclass in second class is without calcining in advance, and the organic matter in the sour molten reaction pair kaolin does not have the ability of removing.As Zhang Qichun etc. at " inferior kaolinic cause the research of look factor " " Chengdu University of Technology's journal " 22 (3): record and narrate in 52,1995, these two kinds of factors all can influence the whiteness of white carbon black product.Although expressed TiO with following reaction formula in above-mentioned " kaolin prepares method for white carbon black research " document 2Sour molten reaction has taken place in the molten process of acid:
But,, can think that dilute sulphuric acid that the author of " kaolin prepare method for white carbon black research " document is used and hydrochloric acid are to the TiO in the kaolin based on following reason 2Mineral do not have perceptible solute effect: at first, industrial practice shows that at the 1979:P27 of " titanium metallurgy " " metallurgical industry press ", P57 is described as Mo Wei etc., except that hydrofluoric acid, and TiO 2Be insoluble in other diluted mineral acid; The vitriol oil of heat could dissolve TiO 2, generate TiOSO 4TiO 2Should just can be converted to TiCl via the chlorine that adds carbon or other chlorizating agent chlorination under>800 ℃ 4Secondly, at TiO 2Content is 0.37% kaolin, carry out bisgallic acid and handle in succession by " kaolin prepares method for white carbon black research " described method of document, can destroy kaolinic crystalline structure, but as described in above-mentioned " inferior kaolinic cause the research of look factor ", be mixed in the interior TiO of kaolin 2Component is failed by used acid dissolving, and it is retained in the siliceous product that is finally obtained with accumulative means, and the khaki color of titanium mineral has reduced the whiteness of gained white carbon black product.
From kaolin, extract the calcination reaction technology of aluminium, U.S. Pat 4342729 Method forObtaining Alumina From Clays (clay is produced method of alumina) and Chinese patent CN1072656A " production method of aluminium hydroxide " are arranged.This two patent is a purpose to obtain aluminum oxide from clay aluminium silicate minerals such as (comprising kaolin) all.US4342729 obtains aluminiferous sulfuric acid double salt, silicon-dioxide and unreacted remaining kaolin via calcining aluminium silicate mineral and the vitriol of basic metal or ammonium or the dry mixture of hydrosulfate; With water or alkali lye solubilizing reaction product, more after filtering, solid filter cake is mainly silicon-dioxide and unreacted kaolin, is settled out the hydration aluminum oxide from filtrate; The calcining hydrated aluminum oxide obtains the aluminum oxide product.Because in this reaction process, the extraction yield of aluminum oxide only be in the protokaolin aluminum oxide 70%~80%, other 20%~30% remaining unreacted kaolin and part iron, titanium mineral are retained in the solid filter cake, make that the siliceous filter cake of solid that is obtained only can be as the raw material of firing ceramics, economic worth is very low.The method of CN1072656A is similar to US4342729.
Given this, the object of the present invention is to provide the calcining and converting reaction process method with preparing white carbon with clay mineral of a kind of whiteness that can improve white carbon black and amorphousness characteristic thereof.
It is raw material that the present invention adopts clay mineral, mix with solid reactants, through pulverizing, calcining, water-dispersion-dissolving, filtering separation, oven dry, make white carbon black, 1: 3 by weight proportion~5 batchings in preparation process, calcining temperature is controlled at 360~750 ℃, calcination time was controlled at 0.5~24 hour, the iron that makes the aluminium matter component in solid reactants and the clay mineral lattice and coexist with clay mineral, titanium oxide reacts, generation has water-soluble and is easy to sulfuric acid double salt and/or the vitriol separated after dissolving, and staying water-fast amorphous silica is that white carbon black is realized its purpose.
Calcining and converting reaction process with preparing white carbon with clay mineral of the present invention has following processing step:
1, with clay mineral and solid reactants, 1: 3 by weight proportion~5 prepare burden, are crushed to granularity less than 100 orders, 360~750 ℃ of following calcinings of temperature 0.5~24 hour, obtain containing aluminiferous sulfuric acid double salt and/or Tai-Ace S 150, with the calcined material of amorphous silica, above-mentioned solid reactants is the vitriol of ammonium or the hydrosulfate or the alkali-metal hydrosulfate of ammonium;
2, add water-dispersion, dissolving calcined material, obtain containing the suspension of the amorphous silica of the aluminiferous sulfuric acid double salt of dissolved and/or Tai-Ace S 150 and dispersion suspension;
3, filtering suspension liquid obtains aluminiferous sulfuric acid double salt and/or Tai-Ace S 150 from filtrate, filter cake obtains white carbon black through washing, oven dry.
Above-mentioned clay mineral is kaolinite clay mineral or illite clay mineral or contains iron, titanium oxide and organic above-mentioned clay mineral raw material.
The above-mentioned clay mineral and the grinding particle size of solid reactants are less than 200 orders.
In the above-mentioned step 2 the pH value of water adjust to≤1.
With above-mentioned processing step, the X ray diffracting spectrum of the white carbon black that makes is typical amorphousness feature, and the whiteness of white carbon black is 95%, density≤0.11g/ml, and specific surface area is 342m 2/ g.
Part by weight in the inventive method, grinding particle size, calcining temperature, calcination time are key parameter.Wherein, the type of specifically selecting the kind, grinding particle size and the used reagent that depend on the raw clay mineral for use of part by weight.When with kaolin being raw material, grinding particle size during less than 200 orders, adopt kaolin: the part by weight of ammonium sulfate is 1: 3, can obtain the amorphous silica product via present method.Be raw material, grinding particle size during less than 200 orders with the illite clay, adopt illite: the part by weight of ammonium sulfate is 1: 3, and the white carbon black product that obtains has reached higher purity and whiteness, and its reason is that illitic aluminium content is lower than kaolinite.Solid materials after the pre-mixing is pulverized, and its effect not only is to reduce the granularity of material particles, and can also improve the mixing uniformity of raw material and reagent two class solid materialss, helps carrying out smoothly of calcining and converting reaction.Therefore the grinding particle size overstriking during for example less than 100 orders, can make the conversion reaction of feed particles nuclear portion be difficult for carrying out thoroughly, wants the usage ratio of corresponding raising reagent, also can be transformed with the lattice aluminium of guaranteeing former clay particle nuclear portion.When being reagent with the hydrosulfate, the usage ratio of reagent can be less than the similar occasion that with ammonium sulfate is reagent.When surmounting suitable usage ratio, when further increasing the consumption of solid reactants, reaction result is had no adverse effects.The selection principle of calcining temperature is: when being reagent with ammonium sulfate and/or monoammonium sulfate, calcining temperature preferably is higher than 500 ℃, so that the exsiccated ammonium alum double salt that generates in the reaction process changes simple vitriol into, the water-soluble reaction that helps is subsequently carried out smoothly; When adopting alkali-metal hydrosulfate to be reagent, because the temperature stability of the sulfuric acid double salt of basic metal-aluminium that conversion reaction generated, row raising calcining temperature also is difficult for changing into simple vitriol again after double salt forms, therefore, when the organic content in the raw clay can be ignored, the calcining temperature that is adopted only need be higher than double salt and generate temperature and get final product, promptly 〉=360 ℃.Calcination time is different with the bed thickness of calcining materials, is as the criterion with the transformation efficiency of the lattice aluminium that guarantees clay mineral.Reach after the suitable calcination time, row prolongs again, and is little to the reaction result influence.
The present invention prepares white carbon black by calcining and converting reaction from clay mineral, simultaneously with the aluminium matter component in the aluminium salt form recycling clay mineral, used solid reactants is the vitriol of ammonium or the hydrosulfate or the alkali-metal hydrosulfate of ammonium, and the preparation process of product is as follows:
With remove in advance the clay of detrital mineral and quantitative solid reactants in the material uniform mixing, mixture preferably is crushed to less than 200 orders.When increasing the solid reactants consumption, also can reduce to pulverize requiring to than coarsness, as less than 100 orders.This compound is placed calcining in the stove, in this calcination process, control calcining temperature>360 ℃, calcination time>30 minute, solid reactants and clay mineral react, and make clay mineral be converted into aluminium ammonium double salt and/or Tai-Ace S 150 or aluminium-basic metal double salt, and amorphous silica.Simultaneously, former tax exists iron, the titanium oxide particulate on clay mineral grain surface that similar sulfuric acid double salt reaction also takes place, and is transformed into to consist of MFe (SO 4) 3And M 2TiO (SO 4) 2Salt, they are all water-soluble, can remove through follow-up water-soluble processing.Like this, when calcining, remove the main reaction of the structure that the destruction clay mineral takes place, the lattice aluminium that is about in the clay mineral is converted into beyond the aluminum soluble salt, also iron, titanium etc. is caused colored foreign and be converted into solvend, solved the removal problem that existing liquid-solid phase reacts the titanium mineral that can not handle.Work as preferred reaction conditions, adopt clay mineral and solid reactants 1: 3 by weight proportion~5 batchings, calcining temperature is controlled at 360~750 ℃, when calcination time is controlled at more than 0.5 hour, main reaction is carried out thoroughly, the conversion of iron, titanium oxide is very complete.With water-dispersion-dissolving calcinate, the pH value of dissolving water is adjusted to≤1, can suppress the hydrolysis reaction of metal ion, the dissolving of assurance metallic salt is carried out smoothly.After the dissolving fully, separate, solution and siliceous micro mist based on aluminium salt are separated from each other out via solid-liquid.The filter cake that siliceous micro mist is formed gets fluffy white micro mist after washing, drying, be the white carbon black product; From with aluminium salt being recyclable aluminum oxide or aluminium hydroxide the filtrate of main component.
Compared with the prior art the present invention has following obvious advantage and unusual effect.
One, the calcining and converting reaction mode of the inventive method employing, preferred reaction conditions, with clay mineral and solid reactants 1: 3 by weight proportion~5 batchings, be crushed to granularity and be controlled at 360~750 ℃, calcination time less than 100 orders, calcining temperature and be controlled at 0.5~24 hour, aluminium matter component in the clay mineral can be bordering on and fully be converted into the solubility salt, simultaneously iron, the titanium mineral that is mingled with in the clay mineral also is transformed into the solubility salt; The amorphous silica that obtains after calcining, both water insoluble, also be insoluble to other acid except that hydrofluoric acid, thereby can be separated via follow-up solubilizing reaction and above-mentioned soluble salt easily, thereby silicon components and al composition and impurity are separated.Present method can reclaim aluminum oxide or aluminium hydroxide from clay mineral, again because can fully remove aluminium matter, organic matter and iron, titanium mineral from clay mineral, obtain the white carbon black of whiteness height, amorphousness excellent, therefore has the advantage of good economy performance.
Two, the inventive method adopted raw clay mineral and solid reactants are solid, be convenient to mix mutually and pulverize through mechanical effect, thereby can in calcining, react, and the granularity of pulverizing is more little, mixing is even more, to make calcining and converting reaction be easy to carry out, therefore the white carbon black that helps obtaining to have high whiteness and amorphousness characteristic.
Three, the above-mentioned preferred reaction conditions of the inventive method the iron in the clay mineral, titanium mineral and organic matter are had good removal effect, and existing liquid-solid phase reaction method is to titanium mineral and organic no removal ability.Therefore, the inventive method far surpasses the molten reaction of existing acid to the adaptability of clay mineral raw material.For example to a kind of shore deposit kaolin of poor quality, when adopting the sour molten treatment process of hydrochloric acid behind above-mentioned " kaolin prepares method for white carbon black research " described first sulfuric acid of document, the whiteness of gained white carbon black is 81% only, and yellow chrominance reaches 5.6%; And use the inventive method preparation, the whiteness of the white carbon black that obtains is 95%, yellow chrominance 3%.Therefore the inventive method has widely and can handle the advantage of inferior raw material to the subject range of raw material, has the utilization of resources and is worth.
Four, use present method to transform the white carbon black product that kaolin obtained and be amorphousness, on its X ray diffracting spectrum, only occur one between 2 θ=15~29 ° and be bordering on symmetric mild diffraction peak, do not have any sharp-pointed diffraction peak in addition and occur, this is the diffractive features of amorphousness silicon-dioxide; Little individuality of the white carbon black that obtains is false hexagonal flake form, and is similar to former kaolinic form, size, shows in reaction process, follows the extracting of lattice aluminium, and when making siliceous component in the kaolinite structure decrystallized, still kept the form of former kaolinite individuality; Footpath/the thickness rate of the little individuality of product>16, this Gao Jing/thickness rate form and amorphousness feature still remain unchanged after being heated to 1000 ℃, give this white carbon black product with outstanding strengthening the property and the high temperature use properties; Density≤the 0.11g/ml of product, analog value 0.23~the 0.24g/ml of the white carbon black that is significantly less than the conventional liquid phase white carbon black described in above-mentioned " kaolin system aluminium chlorohydroxide and white carbon black " and " producing the experimental study of white carbon black with kaolin " two literary compositions and makes from kaolin through the molten reaction of acid, the specific surface area of the product that present method is produced reaches 342m 2/ g, pore volume 0.5ml/g, median size 0.5 μ m has reached the level of gas-phase silica.According to experiment, when transforming the illite clay mineral with present method, the white carbon black product that obtains has and transforms identical typical amorphousness diffractive features and the high whiteness of white carbon black that kaolin obtains, and is only variant with the difference of hyle on form, particle diameter.
Below, the invention will be further described to use embodiment again.
Embodiment 1
A kind of calcining and converting reaction process of the present invention with preparing white carbon with clay mineral, its processing step is as follows:
With kaolin and solid reactants industrial sulphuric acid ammonium, 1: 3.5 by weight proportion batching with its uniform mixing, is crushed to less than 200 orders.Put mixture in retort furnace, control heat-up rate be 500 ℃/hour, be raised to 560 ℃ after, constant temperature 2 hours takes out in retort furnace, reduces to room temperature.
In this calcination process, when temperature be raised to 〉=300 ℃ the time, ammonium sulfate generation decomposition reaction generates monoammonium sulfate:
When temperature further raise, monoammonium sulfate destroyed thereby kaolin crystal is decomposed with the kaolinic lattice aluminium generation sulfuric acid double salt reaction in its high reaction activity and the solid mixt.In this process, form original kaolinic siliceous composition and do not react, but, remain with the amorphous silica form owing to the complete stripping of lattice aluminium makes siliceous composition lose original steric regularity with monoammonium sulfate.
When going the rising temperature of reaction again, NH 4Al (SO 4) 2Double salt decomposes, and stays Al 2(SO 4) 3Because Al 2(SO 4) 3Decomposition temperature be 770 ℃, so the rising of calcination reaction temperature should not surmount this ultimate temperature, so that earlier the aluminum oxide octahedral sheet in the kaolinite structure is converted into aluminiferous sulfuric acid double salt, changes Tai-Ace S 150 again into.
In this calcination process, the similar sulfuric acid double saltization of the aluminium matter component that iron, titanium oxide particulate and monoammonium sulfate take place and kaolin is interior that tax is stored in the kaolin is answered, and changes NH into 4Fe (SO 4) 2And (NH 4) 2TiO (SO 4) 2:
This kaolinite raw material is carried out serial roasting test, and selected maturing temperature is 560 ℃, can make final composition and the whiteness that obtains the white carbon black product all reach optimum value.Under this temperature, the double salt of iron content, titanium can take place and the similar decomposition reaction of aluminium ammonium double salt, changes simple vitriol Fe into 2(SO 4) 3, TiOSO 4
With the calcinate that water-dispersion is taken out in the retort furnace, stir of aluminium, iron, the titanium salt class dissolving of this suspension system to impel calcining to generate, insoluble sheet amorphous silica is suspended in the solution.For preventing the metallic salt hydrolysis, the pH value with a small amount of dilute sulphuric acid adjustment dissolving water maintains pH≤1 in the process.After the dissolving fully, with the gained suspension filtered.Filter cake washes with water to neutrality, and oven dry gets fluffy white powder, is the white carbon black product.
From the filtrate of filtering gained, reclaim aluminum oxide or aluminium hydroxide.
Present embodiment is found the test that the reaction conditions of kaolinic above-mentioned calcining and converting reaction carries out:
(1) when using ammonium sulfate as solid reactants, because therefore the solubleness of exsiccated ammonium alum double salt, adopt higher calcining temperature less than Tai-Ace S 150, changing double salt is simple vitriol, can make water-soluble processing subsequently be easy to carry out thoroughly.
(2) under selected maturing temperature, the organic matter of carrying secretly in the clay mineral can decompose gasification, volatilizees away from calcinate.
(3) this calcining and converting reaction does not need inert environments, and whether the charge crucible seals, and final obtained product character is not had obvious influence.
(4) calcinate is fluffy soft block, and exerting pressure slightly is pulverizable, and this helps the dissolving of water to the salt in the calcinate.
(5) after leaving standstill, microplate shape silicon-dioxide is easy to settle down from solution, is convenient to filter and washing.
After handling with the method for the invention, the chemical ingredients of institute's white carbon black product that obtains and kaolin raw material contrasts as following table:
Composition (%) SiO 2 Al 2O 3 Fe 2O 3 TiO 2 Na 2O K 2O
The kaolin raw material 44.6 37.0 2.5 1.2 0.32 0.07
White carbon black product (butt) 99.1 0.31 0.02 0.05 0.10 <0.01
The used kaolin raw material of present embodiment turns to be yellow because of iron content, belongs to kaolin inferior.When measuring kaolinic whiteness, the absolute reflectance with blue light (wavelength is 457nm) is designated as whiteness usually.When measuring the whiteness of using present method obtained product, adopt the whiteness souvenir symbol R of Britain 457, the absolute reflectance of blue light (wavelength is 457nm) is designated as R 457Whiteness, i.e. whiteness.After present method processing, the R of the white carbon black product that obtains 457Whiteness is 95%, yellow chrominance 2.7%, tap density 0.11g/ml, specific surface area 342m 2/ g.Present method is to the extraction rate reached 99% of aluminium matter component in the kaolin.
Embodiment 2
A kind of calcining and converting reaction process with preparing white carbon with clay mineral of the present invention is a raw material with Miyi, Sichuan illite clay, and solid reactants is NaHSO 4And KHSO 4Wait molar mixture, the part by weight of illite clay and solid reactants is 1: 3.Raw material and solid reactants are carried out mechanically mixing, and be crushed to less than 200 orders.Mixture is placed in the retort furnace calcining 2 hours, 400 ℃ of calcining temperatures.With calcinate that water-dispersion is obtained, be aided with to stir and impel the sulfuric acid double salt dissolving that generates in the calcining conversion process complete.Suspension is carried out solid-liquid separation,, get white carbon black, its SiO the oven dry of obtaining filter cake 2Content is 98.1%, R 457Whiteness is 94.2%.
Embodiment 3
A kind of calcining and converting reaction process of the present invention with preparing white carbon with clay mineral, the selecting for use and preparing and calcine of its raw material, solid reactants-dissolution process is similar to embodiment 1, but grinding particle size is less than 100 orders, and the part by weight of raw material and solid reactants is 1: 5.The SiO of the final white carbon black that obtains 2Content is 98.3%, R 457Whiteness is 93.7%.
Embodiment 4
A kind of calcining and converting reaction process with preparing white carbon with clay mineral of the present invention, the selecting for use and preparing and calcine of its raw material, solid reactants-dissolution process is similar to embodiment 1, but the calcination time that is adopted is 24 hours.The SiO of the final white carbon black product that obtains 2Content is 99.1%, R 457Whiteness is 94.6%.
Embodiment 5
A kind of calcining and converting reaction process with preparing white carbon with clay mineral of the present invention is a raw material with Suzhou kaolin, and the selecting for use, prepare and calcine of its raw material and solid reactants-dissolution process is similar to embodiment 1, but the temperature of reaction that is adopted is 750 ℃.The SiO of the final white carbon black that obtains 2Content is 98.7%, R 457Whiteness is 94.0%.

Claims (7)

1, with the calcining and converting reaction process of preparing white carbon with clay mineral, it is characterized in that following processing step is arranged:
1) with clay mineral and solid reactants, 1: 3 by weight proportion~5 prepare burden, are crushed to granularity less than 100 orders, 360~750 ℃ of following calcinings of temperature 0.5~24 hour, obtain containing aluminiferous sulfuric acid double salt and/or Tai-Ace S 150, with the calcined material of amorphous silica, above-mentioned solid reactants is the vitriol of ammonium or the hydrosulfate or the alkali-metal hydrosulfate of ammonium;
2) add water-dispersion, dissolving calcined material, obtain containing the suspension of the amorphous silica of the aluminiferous sulfuric acid double salt of dissolved and/or Tai-Ace S 150 and dispersion suspension;
3) filtering suspension liquid obtains aluminiferous sulfuric acid double salt and/or Tai-Ace S 150 from filtrate, filter cake obtains white carbon black through washing, oven dry.
2, technology according to claim 1 is characterized in that said clay mineral is kaolinite clay mineral or illite clay mineral or contains iron, titanium oxide and organic above-mentioned clay mineral raw material.
3, technology according to claim 1 and 2, the granularity that it is characterized in that said clay mineral and solid reactants is less than 200 orders.
4, technology according to claim 1 and 2 is characterized in that said step 2) in the pH value of water adjust to≤1.
5, technology according to claim 3 is characterized in that said step 2) in the pH value of water adjust to≤1.
6, technology according to claim 1 and 2 is characterized in that the X ray diffracting spectrum of said white carbon black is typical amorphousness feature, and the whiteness of white carbon black is 95%, density≤0.11g/ml, and specific surface area is 342m 2/ g.
7, technology according to claim 3 is characterized in that the X ray diffracting spectrum of said white carbon black is typical amorphousness feature, and the whiteness of white carbon black is 95%, density≤0.11g/ml, and specific surface area is 342m 2/ g.
CN98112175A 1998-08-07 1998-08-07 Calcining and converting reaction process of preparing white carbon with clay mineral Expired - Fee Related CN1102126C (en)

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CN1046507A (en) * 1989-04-21 1990-10-31 李抚立 Kaolin is produced the method for poly aluminium chloride and white carbon black

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US4342729A (en) * 1979-07-26 1982-08-03 Jesus Martinez Lope Method for obtaining alumina from clays
CN1046507A (en) * 1989-04-21 1990-10-31 李抚立 Kaolin is produced the method for poly aluminium chloride and white carbon black

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