CN110283479A - A kind of compound sericite of ultrawhite and preparation method thereof - Google Patents

A kind of compound sericite of ultrawhite and preparation method thereof Download PDF

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CN110283479A
CN110283479A CN201910711256.6A CN201910711256A CN110283479A CN 110283479 A CN110283479 A CN 110283479A CN 201910711256 A CN201910711256 A CN 201910711256A CN 110283479 A CN110283479 A CN 110283479A
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sericite
suspension
solution
ultrawhite
preferable
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CN110283479B (en
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张宏
张斌
裸伍拉哈
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Sichuan Saixin Material Science And Technology Co Ltd
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Sichuan Saixin Material Science And Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3045—Treatment with inorganic compounds
    • C09C1/3054—Coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043—Drying, calcination
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating

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  • Organic Chemistry (AREA)
  • Cosmetics (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

A kind of compound sericite product of ultrawhite is provided, it includes sericite as substrate or core and the titanium dioxide layer, magnesium oxide layer and the silicon dioxide layer that successively coat on sericite surface.The method for preparing the compound sericite product of the ultrawhite from the grey sericite of low whiteness is also provided.

Description

A kind of compound sericite of ultrawhite and preparation method thereof
Technical field
The natural sericite (such as grey sericite) that the present invention relates to a kind of from low whiteness prepares the compound sericite of ultrawhite And preparation method thereof, belong to new inorganic non-metallic materials field.
Background technique
Sericite is a kind of potassium aluminium silicate mineral with stratiform or sheet output, is a subspecies of muscovite mine, is With the muscovite of microfine output, it is all physics chemistry characteristic for having muscovite: excellent insulating properties, and good chemistry is steady Qualitative (room temperature is also insoluble in alkali insoluble in acid), heat-resisting quantity (800 DEG C or more are just dehydrated, and become opaque), radius-thickness ratio is big, Any surface finish, feel is fine and smooth smooth soft, has the sliding gloss of bright silk, and monomer granularity is in finely squamose between 2-10um. Its good dispersion, hiding rare is good, and granularity is moderate, has similar kaolinic characteristic；It is strong carefully to slide sense, adhesive force is strong, and has Talcum characteristic, therefore, sericite tool have been widely used.Fine and smooth smooth, good skin sense, and be to have ultraviolet shielding function and use In cosmetics filler；Laminated structure has humidification and is used for enhancing modification of plastic, can greatly improve the rigidity of plastic products And bending resistance；Laminated structure, to have good water vapor rejection performance and be used for anticorrosive paint；With reinforcing effect, It can partially replace carbon black, white carbon black for reinforcing rubber；Gloss is bright fine and smooth, yellowing-resistant and be used for Paper Coating；Rich potassium can have Effect reduces fusing point, and is used for ceramics, welding rod etc., it is insufficient and one, although these purposes, the different use of sericite are utilized Characteristic, but have a common prescription to sericite --- whiteness, it is desirable that the higher the better for whiteness, and whiteness is generally required to be greater than 75, And sericite, as a kind of mineral generated naturally, ore-forming setting condition is multifarious, is associated with coloring mineral or has disseminated cause Grey is presented in the sericite of color ion, is commonly called as grey sericite, and natural whiteness generally all only has 60 or so, the reserves of this kind of ore It is huge, due to whiteness it is too low and without application value.Therefore, the whiteness of grey sericite is improved, realizes low value or without application value Sericite ore resource high added value, be the key core technologies problem of the sector.At present it is not yet found that specialised literature Or technical patent solves the problems, such as such.
Summary of the invention
In view of the deficiencies of the prior art, inventor conducts in-depth research, as a result, it has been found that, by grey sericite in powder Surface cladding multilayer whiteness is high, covering power is good, stable chemical performance oxide, obtains a kind of compound sericite of ultrawhite.
The purpose of the present invention is such as grey sericites of the sericite using low whiteness to prepare the compound thin,tough silk of ultrawhite of high whiteness Mica.
According to the first embodiment of the present invention, provide ultrawhite compound sericite, it includes the thin,tough silk as substrate or core Titanium dioxide layer, the oxygen mica (such as natural sericite or natural grey sericite) and successively coated on sericite surface Change magnesium layer and silicon dioxide layer.
Generally, as substrate or core come using sericite (such as natural sericite or natural grey sericite) raw material The average grain diameter of powder be 0.5-60 μm, preferably 0.8-50 μm, more preferable 1-40 μm, more preferable 1.5-35 μm, more preferably 1.8-30 μm, more preferable 2-20 μm, more preferable 2-15 μm.
It is preferred that the sericite raw material used in the present invention as substrate or core be whiteness it is lower (such as whiteness is lower than 60, For example, whiteness is 30,35,40 or the powder of natural sericite (such as grey sericite) 55) in 20-60 range, such as whiteness Material.
It is preferred that in the compound sericite of ultrawhite of the invention, titanium dioxide layer is relative to sericite (such as grey thin,tough silk cloud It is female) weight ratio for the weight of powder substrate is 3-30%, preferably 5-25%, 10-28%, more preferable 15-20%.
It is preferred that magnesium oxide layer is relative to sericite (such as grey sericite) in the compound sericite of ultrawhite of the invention Weight ratio for the weight of powder substrate is 5-50%, preferably 10-40%, 15-35%, more preferable 20-30%；And/or
It is preferred that in the compound sericite of ultrawhite of the invention, silicon dioxide layer is relative to sericite (such as grey thin,tough silk cloud It is female) weight ratio for the weight of powder substrate is 0.1-10%, preferably 0.5-9.0%, 1-8%, more preferable 1.5-7%.
According to the second embodiment of the present invention, the method for preparing the compound sericite of above-mentioned ultrawhite, this method are also provided The following steps are included:
(1) sericite raw base substrate is stirred with deionized water, obtains sericite suspension；
(2) using titanium salt solution corresponding with titanium dioxide to the sericite cladding titanium dioxide in sericite suspension Layer；
(3) sericite in the suspension for utilizing magnesium salt solution corresponding with magnesia to obtain step (2) is further Coated magnesium oxide layer；
(4) suspension obtained using the solution of silicate corresponding with silica or metasilicate for step (3) In the further coated silica layer of sericite；With
(5) suspension obtained to step (4) is filtered, washs, dries and calcines, and obtains having the super of ultrawhite effect Bai Fuhe sericite in powder.
More specifically, the present invention provides a kind of method for preparing the compound sericite of above-mentioned ultrawhite, and this method includes following Step:
(1) the sericite raw base substrate of 100 parts by weight is stirred with deionized water, acquisition solid-to-liquid ratio is 1:(4- 35), preferably 1:(5-30), more preferable 1:(7-25), more preferable 1:(10-20) sericite suspension；
(2) by the suspension of step (1) be warming up to 40-100 DEG C (preferably 50-90 DEG C, preferably 60-85 DEG C, more preferably 70-80 DEG C) temperature, and be adjusted with acid the pH value of suspension in 0.5-5.5 range, preferably in 1-5 range, more preferably in 1.5- 4 ranges, more preferably in 1.5-3.5 range；Then, titanium salt solution corresponding with titanium dioxide is added into suspension to be reacted And continue to stir the suspension (such as -5 hours 3 minutes, such as 30-40 minutes) after titanium salt solution charging terminates, so as to Obtain the suspension for having coated the sericite of titanium dioxide layer on the surface containing one kind；Wherein, the additive amount of titanium salt solution is answered Should so that in the compound sericite product of ultrawhite weight of the titanium dioxide layer relative to sericite (such as grey sericite) powder substrate Weight ratio for amount is 3-30% (preferably 5-25%, 10-28%, more preferable 15-20%)；Preferably, add above-mentioned It keeps the pH of suspension stable or basicly stable with alkali in material and reaction process, such as keeps pH stable in 0.5-5.5 range (preferably in 1-5 range, more preferably in 1.5-4 range, more preferably in 1.5-3.5 range)；
(3) by step (2) suspension obtained be maintained at 40-100 DEG C (preferably 50-90 DEG C, preferably 60-85 DEG C, more Preferably 70-80 DEG C) at a temperature in the range of, it is (preferably 5.5-13.0, more excellent that the pH of suspension is adjusted to 4.5-14.0 with alkali It is selected as 6.0-12.5, more preferably 7.0-12.0, more preferably 8.0-11.0), then added and magnesia pair into suspension The magnesium salt solution answered carries out reaction and to continue to stir the suspension after magnesium salt solution charging terminates (such as 3 minutes -5 small When, such as 30-40 minutes), magnesia has further been coated on the coated by titanium dioxide layer of sericite containing a kind of to obtain The suspension of the sericite of layer；Wherein, the additive amount of magnesium salt solution should make the magnesia in the compound sericite product of ultrawhite Weight ratio of the layer for the weight of sericite (such as grey sericite) powder substrate be 5-50% (preferably 10-40%, 15-35%, more preferable 20-30%)；Preferably, suspension is kept with alkali and acid respectively in above-mentioned charging and reaction process PH it is stable or basicly stable, such as keep pH stable 4.5-14.0 (preferably 5.5-13.0, more preferably 6.0-12.5, More preferably 7.0-12.0, more preferably 8.0-11.0)；
(4) by step (3) suspension obtained be maintained at 40-100 DEG C (preferably 50-90 DEG C, preferably 60-85 DEG C, more Preferably 70-80 DEG C) at a temperature in the range of, the pH of the suspension is adjusted to 4.5-12.0 (preferably 5.0- with acid or alkali 11.5,6.0-11, more preferably 6.5-10.0, more preferably 7.0-9.0 are more preferably)；Then the addition and two into suspension The solution of the corresponding silicate of silica or metasilicate is reacted, wherein the addition of the solution of silicate or metasilicate Amount should make in the compound sericite product of ultrawhite silicon dioxide layer relative to sericite (such as grey sericite) powder substrate Weight for weight ratio be 0.1-10% (preferably 0.5-9.0%, 1-8%, more preferable 1.5-7%), it is preferred that It keeps the pH of suspension stable or basicly stable with alkali and acid respectively in the charging and reaction process, such as pH stable is kept to exist 4.5-12.0 (preferably 5.0-11.5, more preferably 6.0-11, more preferably 6.5-10.0, more preferably 7.0-9.0)；And After the addition of silicate or the solution of metasilicate terminates, by with alkali adjust suspension pH value 7.5-11 (preferably 8.0-10, more preferable 8.5-9.5) continue to stir the suspension (such as -5 hours 3 minutes, such as 30-40 minutes) in range, so as to Obtain the suspension for containing a kind of sericite that silicon dioxide layer has further been coated on the magnesia clad of sericite；With
(5) suspension obtained to step (4) is filtered, washs, dries and calcines, and obtains having the super of ultrawhite effect Bai Fuhe sericite in powder product.The whiteness of the compound sericite in powder product of the ultrawhite is higher than 75, more preferably higher than 80, more preferably higher than 84。
It is preferred that the acid for adjusting pH is to use in the form of a solution, the acid solution is molten selected from hydrochloric acid solution, sulfuric acid One of liquid, phosphoric acid solution or nitric acid solution are a variety of.
It is preferred that the alkali for adjusting pH is to use in the form of a solution, the aqueous slkali is selected from sodium hydroxide solution, hydrogen One of potassium oxide solution, sodium carbonate liquor, solution of potassium carbonate, ammonia spirit are a variety of.
It is preferred that titanium salt solution corresponding with titanium dioxide is by selected from TiCl4、Ti2(SO4)3And TiOSO4One of Or a variety of titanium salts are formed by solution.
It is preferred that magnesium salt solution corresponding with magnesia is by selected from MgSO4、MgCl2With Mg (NO3)2One of or it is more Kind titanium salt is formed by solution.
It is preferred that silicate corresponding with silica or metasilicate solution are by selected from Na2SiO3、K2SiO3With MgSiO3One of or a variety of salt be formed by solution.
It is preferred that in the above-mentioned methods, drying is at 80-180 DEG C (preferably 100-150 DEG C, 110-130 DEG C more preferable) At a temperature of dry -6 hours 1 hour, it is 3-5 hours more preferable.
It is preferred that calcining is the temperature lower calcination 5 at 500 DEG C -900 DEG C (preferably 600-800 DEG C, 650-750 DEG C more preferable) Minute~30min, it is 10-15 minutes more preferable.
In this application, it " keeps the pH of suspension stable or basicly stable " to refer to: the pH stable of suspension being kept to exist In ± 1 range for setting pH value, more preferably stablize in ± 0.5 range of setting pH value.
The present invention provides a kind of compound sericite of ultrawhite, it is characterized in that successively coating two on its surface using sericite as core Titanium oxide, magnesia, silica, whiteness are more than or equal to 75, have preferable covering, stable chemical property, bright and soft The gloss of sum and preferable function of shielding ultraviolet radiation.
Wherein the partial size of grey sericite in powder has 1-10 μm, 1-15 μm, 10-30 μm, 10-60 μm, preferably 1-10 μm, 1-15 μm, 10-30 μm of grey sericite in powder, more preferable 1-15 μm of grey sericite in powder is as substrate.
Wherein titanium dioxide, magnesia, the respective weight of silica oxides layer are as follows:
Titanium dioxide is 3-30%, preferably 5-25%, 10-28% relative to the weight of grey sericite in powder substrate, more excellent Select 15-20%；
Magnesia is 5-50%, preferably 10-40%, 15-35% relative to the weight of grey sericite in powder substrate, more preferably 20-30%.
Silica is 0.1-10%, preferably 0.5-9.0%, 1-8% relative to the weight of grey sericite in powder substrate, more It is preferred that 1.5-7%；
It is a further object of the present invention to provide a kind of preparation methods for preparing the compound sericite of ultrawhite, and steps are as follows:
(1) 100 parts of substrates are mixed with deionized water, forming solid-to-liquid ratio is 1:(5~25), preferred 1:(5~20), more excellent Select 1:(10~20) suspension, stir evenly.
(2) 60-90 DEG C, preferably 65-85 DEG C, more preferably 70-80 DEG C are warming up to.The pH of suspension is adjusted with acid solution To 0.5-5.0, preferably 1.0-4.0, more preferably 1.5-3.5, the titanium salt corresponding with titanium dioxide that concentration is 2mol/L is added Solution, the specific gravity for being added to titanium dioxide relative to substrate is 15-20%, can stop feeding, and keeps pH value constant with aqueous slkali. Constant temperature stirs (such as 5 minutes~1 hour, preferably from about 40 minutes, more preferably 30 minutes) after stopping charging；
(3) keep it is above-mentioned temperature-resistant, with aqueous slkali by the pH of suspension be adjusted to 4.0-14.0, preferably 6.0-12.0, More preferably 8.0-11, into solution be added dropwise mass fraction be 5%-35%, preferably 10%-30%, more preferable 15-25% with The corresponding magnesium salt solution of magnesia, the specific gravity for being added to magnesia relative to substrate is 20-30%, can stop feeding, use alkali soluble Liquid and acid solution keep solution ph constant simultaneously.It reacts to the form and aspect of required ultrawhite, constant temperature stirs 30 minutes after stopping charging.
(4) pH of suspension is adjusted to 5.0-11.0, preferably 6.0-10.0, more preferably 7.0- with acid or aqueous slkali 9.0, addition mass fraction is the silicon salt corresponding with silica of 5%-35%, preferably 10%-30%, more preferable 15-25% Solution keeps pH value constant with aqueous slkali and acid solution, and after charging, adjusting pH with aqueous slkali is 8.0~10.0, and constant temperature stirs Mix (such as 5 minutes~1 hour, preferably from about 35 minutes)；
(5) solution obtained to step (4) is filtered, washs, dries, calcines, and obtains having the super of ultrawhite effect Bai Fuhe sericite in powder.
Wherein, the solution of the optional hydrochloric acid of the acid solution, sulfuric acid and/or their any combination；
The solution of the optional sodium hydroxide of alkali, ammonium hydroxide, sodium carbonate in the aqueous slkali and/or their any combination, example If aqueous slkali is the aqueous solution of sodium hydroxide or ammonium hydroxide or carbonic acid sodium, such as 5-30% sodium carbonate liquor or 5~30% ammonium hydroxide.
The corresponding titanium salt solution of the titanium dioxide can be TiCl4、Ti2(SO4)3、TiOSO4And/or theirs is any Combined solution.
The corresponding magnesium salt solution of the magnesia can be MgSO4、MgCl2、Mg(NO3)2And/or their any group The solution of conjunction.
The corresponding silicon salt solution of the silica can be Na2SiO3、K2SiO3、MgSiO3And/or theirs is any Combined solution.
Drying is, for example, drying 1 hour~6 hours at preferably from about 100-150 DEG C, more preferably in 110- at 80-180 DEG C It is about 3-5 hours dry at 130 DEG C.
Calcining is, for example, 5 minutes~30min to be calcined at preferably from about 600-800 DEG C, more preferably from about at 500 DEG C~900 DEG C It is calcined 10 minutes at 650-750 DEG C.
Whiteness >=75 of the powder of the compound sericite of ultrawhite prepared by the present invention, preferably >=78, more preferably >=80.
Advantageous effects of the invention:
The compound sericite in powder of ultrawhite prepared by the present invention be grey sericite in powder surface successively cladding titanium dioxide, oxidation Magnesium, silicon dioxide layer oxide and obtain, by change clad thickness, thus it is possible to vary whiteness effect, this compound thin,tough silk of ultrawhite Mica has fabulous smoothness, and sense of touch is good, strong covering power, stable chemical property, bright and soft gloss and preferably Function of shielding ultraviolet radiation, can be widely applied to car paint, cosmetics, fiber and cloth, ceramics and enamel, household items, In the fields such as synthetic leather, electronics and electrical equipment, ship.
The whiteness of grey thin,tough silk cloud is increased to 75 or more from 60 or so by the compound sericite in powder of ultrawhite of the invention, so that without answering High added value is realized with the grey sericite of value.This product that the cladding of especially multilevel oxide obtains, has Better ultraviolet shielded effect, especially suitable for cosmetics.
Specific embodiment
The present invention is described in further detail technical solution by following examples, but the present invention is not restricted to these implement Example.
Embodiment 1
(1) partial size for weighing 100g grams of dry weight is 1-15 μm of grey sericite in powder, is put into the reaction kettle that volume is 2L, 1200 ml deionized waters are added, stirring is allowed to evenly dispersed at suspension；
(2) this suspension is heated in thermostat water bath, is warming up to 70 DEG C.The pH of suspension is adjusted with hydrochloric acid solution To 2.0, the TiCl that concentration is 2mol/L is added4Solution 110ml (corresponding TiO2Specific gravity relative to substrate grey sericite in powder For that 15%), can stop feeding, keep pH value constant with liquid alkaline solution.Constant temperature stirs 30 minutes after stopping charging；
(3) it keeps above-mentioned temperature-resistant, the pH of suspension is adjusted to 11 with liquid alkaline solution, quality point is added dropwise into solution The MgCl that number is 15%2·6H2O solution 840.8ml (corresponding MgO is 20% relative to the specific gravity of substrate grey sericite in powder), is used Liquid alkaline solution and hydrochloric acid solution keep solution ph constant simultaneously.Constant temperature stirs 30 minutes after stopping charging.
(4) pH of suspension is adjusted to 8.5 with hydrochloric acid solution, addition mass fraction is 15%Na2SiO3·9H2O solution 97.76ml (corresponding SiO2Specific gravity relative to substrate grey sericite in powder is 3%), to keep pH with liquid alkaline solution and hydrochloric acid solution Be worth it is constant, after charging, with liquid alkaline solution adjust pH be 10.0, constant temperature stir 35 minutes)；
(5) solution obtained to step (4) is filtered, washs, 3 hours dry at 120 DEG C, at a temperature of 700 DEG C Calcining 10 minutes, obtains having the compound sericite in powder of the ultrawhite of ultrawhite effect.
Gained sample clad ratio:
Wherein TiO2%=15%, MgO%=20%, SiO2%=3%,
Gained sample whiteness are as follows: the 78 (whiteness of former ash color sericite in powder substrate are as follows: 50)
Embodiment 2
(1) partial size for weighing 100g grams of dry weight is 1-15 μm of grey sericite in powder, is put into the reaction kettle that volume is 2L, 1200 ml deionized waters are added, stirring is allowed to evenly dispersed at suspension；
(2) this suspension is heated in thermostat water bath, is warming up to 70 DEG C.The pH of suspension is adjusted with hydrochloric acid solution To 2.0, the TiCl that concentration is 2mol/L is added4Solution 156.3ml (corresponding TiO2Ratio relative to substrate grey sericite in powder Weight is that 20%), can stop feeding, and keeps pH value constant with liquid alkaline solution.Constant temperature stirs 30 minutes after stopping charging；
(3) it keeps above-mentioned temperature-resistant, the pH of suspension is adjusted to 11 with liquid alkaline solution, quality point is added dropwise into solution The MgCl that number is 15%2·6H2O solution 1120.9ml (corresponding MgO is 25% relative to the specific gravity of substrate grey sericite in powder), Keep solution ph constant simultaneously with liquid alkaline solution and hydrochloric acid solution.Constant temperature stirs 30 minutes after stopping charging.
(4) pH of suspension is adjusted to 8.5 with hydrochloric acid solution, addition mass fraction is 15%Na2SiO3·9H2O solution 131.50ml (corresponding SiO2Specific gravity relative to substrate grey sericite in powder is 4%), to be kept with liquid alkaline solution and hydrochloric acid solution PH value is constant, and after charging, adjusting pH with liquid alkaline solution is 10.0, and constant temperature stirs 35 minutes)；
(5) solution obtained to step (4) is filtered, washs, 3.5 hours dry at 120 DEG C, in 700 DEG C of temperature Lower calcining 10 minutes, obtains having the compound sericite in powder of the ultrawhite of ultrawhite effect.
Gained sample clad ratio:
Wherein TiO2%=20%, MgO%=25%, SiO2%=4%,
Gained sample whiteness are as follows: the 80 (whiteness of former ash color sericite in powder substrate are as follows: 50)
Embodiment 3
(1) partial size for weighing 100g grams of dry weight is 1-15 μm of grey sericite in powder, is put into the reaction kettle that volume is 2L, 1200 ml deionized waters are added, stirring is allowed to evenly dispersed at suspension；
(2) this suspension is heated in thermostat water bath, is warming up to 70 DEG C.The pH of suspension is adjusted with hydrochloric acid solution To 2.0, the TiCl that concentration is 2mol/L is added4Solution 156.3ml (corresponding TiO2Ratio relative to substrate grey sericite in powder Weight is that 20%), can stop feeding, and keeps pH value constant with liquid alkaline solution.Constant temperature stirs 30 minutes after stopping charging；
(3) it keeps above-mentioned temperature-resistant, the pH of suspension is adjusted to 11 with liquid alkaline solution, quality point is added dropwise into solution The MgSO that number is 15%4·7H2O solution 1747.5ml (corresponding MgO is 30% relative to the specific gravity of substrate grey sericite in powder), Keep solution ph constant simultaneously with liquid alkaline solution and hydrochloric acid solution.Constant temperature stirs 30 minutes after stopping charging.
(4) pH of suspension is adjusted to 8.5 with hydrochloric acid solution, addition mass fraction is 15%Na2SiO3·9H2O solution 165.88ml (corresponding SiO2Specific gravity relative to substrate grey sericite in powder is 5%), to be kept with liquid alkaline solution and hydrochloric acid solution PH value is constant, and after charging, adjusting pH with liquid alkaline solution is 10.0, and constant temperature stirs 35 minutes)；
(5) solution obtained to step (4) is filtered, washs, 4 hours dry at 120 DEG C, at a temperature of 750 DEG C Calcining 10 minutes, obtains having the compound sericite in powder of the ultrawhite of ultrawhite effect.
Gained sample clad ratio:
Wherein TiO2%=20%, MgO%=30%, SiO2%=5%,
Gained sample whiteness are as follows: the 84 (whiteness of former ash color sericite in powder substrate are as follows: 50)
Table 1
TiO has successively been coated on the basis of former ash color sericite in powder it can be seen from upper table 12、MgO、SiO2Afterwards, whiteness Increase, and increase with clad ratio, whiteness also increases.

Claims (10)

1. the compound sericite of ultrawhite, it include sericite as substrate or core and successively coated on sericite surface two Titanium oxide layer, magnesium oxide layer and silicon dioxide layer.
2. the compound sericite of ultrawhite according to claim 1, which is characterized in that as substrate or core come using sericite The average grain diameter of the powder of raw material be 0.5-60 μm, preferably 0.8-50 μm, more preferable 1-40 μm, more preferable 1.5-35 μm, More preferably 1.8-30 μm, more preferable 2-20 μm, more preferable 2-15 μm.
3. the compound sericite of ultrawhite according to claim 1 or 2, which is characterized in that sericite raw material is the lower (example of whiteness If whiteness be lower than 60, for example, whiteness is in 20-60 range) grey sericite powder；And/or
Whiteness >=75 of the powder of the compound sericite of ultrawhite, preferably >=78, more preferably >=80.
4. the compound sericite of ultrawhite described in any one of -3 according to claim 1, which is characterized in that in the compound thin,tough silk of ultrawhite In mica, weight ratio of the titanium dioxide layer for the weight of sericite (such as grey sericite) powder substrate is 3- 30%, preferably 5-25%, 10-28%, more preferable 15-20%；And/or
In the compound sericite of ultrawhite, magnesium oxide layer is for the weight of sericite (such as grey sericite) powder substrate Weight ratio be 5-50%, preferably 10-40%, 15-35%, more preferable 20-30%；And/or
In the compound sericite of ultrawhite, silicon dioxide layer is for the weight of sericite (such as grey sericite) powder substrate Weight ratio be 0.1-10%, preferably 0.5-9.0%, 1-8%, more preferable 1.5-7%.
5. the method for preparing any one of -4 compound sericite of ultrawhite according to claim 1, this method includes following step It is rapid:
(1) sericite raw base substrate is stirred with deionized water, obtains sericite suspension；
(2) using titanium salt solution corresponding with titanium dioxide to the sericite cladding titanium dioxide layer in sericite suspension；
(3) sericite in the suspension obtained using magnesium salt solution corresponding with magnesia for step (2) is further coated Magnesium oxide layer；
(4) in the suspension for utilizing the solution of silicate corresponding with silica or metasilicate to obtain step (3) The further coated silica layer of sericite；With
(5) suspension obtained to step (4) is filtered, washs, dries and calcines, and obtains having the ultrawhite of ultrawhite effect multiple Close sericite in powder.
6. according to the method for claim 5 or it is a kind of prepare according to claim 1 any one of -4 the compound thin,tough silk of ultrawhite The method of mica, method includes the following steps:
(1) the sericite raw base substrate of 100 parts by weight is stirred with deionized water, acquisition solid-to-liquid ratio is 1:(4-35), it is excellent Select 1:(5-30), more preferable 1:(7-25), more preferable 1:(10-20) sericite suspension；
(2) suspension of step (1) is warming up to 40-100 DEG C of (preferably 50-90 DEG C, preferably 60-85 DEG C, more preferably 70-80 DEG C) temperature, and be adjusted with acid the pH value of suspension in 0.5-5.5 range, preferably in 1-5 range, more preferably in 1.5-4 model It encloses, more preferably in 1.5-3.5 range；Then, titanium salt solution corresponding with titanium dioxide is added into suspension to be reacted simultaneously And continue to stir the suspension (such as -5 hours 3 minutes, such as 30-40 minutes) after titanium salt solution charging terminates, to obtain Obtain the suspension for having coated the sericite of titanium dioxide layer on the surface containing one kind；Wherein, the additive amount of titanium salt solution should So that weight of the titanium dioxide layer relative to sericite (such as grey sericite) powder substrate in the compound sericite product of ultrawhite For weight ratio be 3-30% (preferably 5-25%, 10-28%, more preferable 15-20%)；
(3) by step (2) suspension obtained be maintained at 40-100 DEG C (preferably 50-90 DEG C, preferably 60-85 DEG C, more preferably It is 70-80 DEG C) at a temperature in the range of, the pH of suspension is adjusted to 4.5-14.0 with alkali and (preferably 5.5-13.0, is more preferably 6.0-12.5, more preferably 7.0-12.0, more preferably 8.0-11.0), it is then added into suspension corresponding with magnesia Magnesium salt solution carry out reaction and continue to stir after magnesium salt solution charging terminates the suspension (such as -5 hours 3 minutes, such as 30-40 minutes), to obtain containing a kind of thin,tough silk for further having coated magnesium oxide layer on the coated by titanium dioxide layer of sericite The suspension of mica；Wherein, the additive amount of magnesium salt solution should make the magnesium oxide layer in the compound sericite product of ultrawhite opposite Weight ratio for the weight of sericite (such as grey sericite) powder substrate is 5-50% (preferably 10-40%, 15- 35%, more preferable 20-30%)；
(4) by step (3) suspension obtained be maintained at 40-100 DEG C (preferably 50-90 DEG C, preferably 60-85 DEG C, more preferably It is 70-80 DEG C) at a temperature in the range of, the pH of the suspension is adjusted to 4.5-12.0 (preferably 5.0-11.5, more with acid or alkali Preferably 6.0-11, more preferably 6.5-10.0, more preferably 7.0-9.0)；Then addition and silica pair into suspension The solution of the silicate or metasilicate answered is reacted, wherein the additive amount of the solution of silicate or metasilicate should make In the compound sericite product of ultrawhite silicon dioxide layer relative to sericite (such as grey sericite) powder substrate weight and The weight ratio of speech is 0.1-10% (preferably 0.5-9.0%, 1-8%, more preferable 1.5-7%)；And in silicate or inclined silicon After the addition of the solution of hydrochlorate terminates, by with alkali adjust suspension pH value 7.5-11 (preferably 8.0-10, more preferably 8.5-9.5) continue to stir the suspension (such as -5 hours 3 minutes, such as 30-40 minutes) in range, to obtain containing one kind The suspension of the sericite of silicon dioxide layer has further been coated on the magnesia clad of sericite；With
(5) suspension obtained to step (4) is filtered, washs, dries and calcines, and obtains having the ultrawhite of ultrawhite effect multiple Close sericite in powder.
7. according to the method described in claim 6, wherein being kept in above-mentioned charging and reaction process with alkali in step (2) The pH of suspension is stable or basicly stable, such as pH stable is kept (preferably in 1-5 range, more preferably to exist in 0.5-5.5 range 1.5-4 range, more preferably in 1.5-3.5 range)；And/or
Wherein in step (3), keep the pH of suspension stable or base with alkali and acid respectively in above-mentioned charging and reaction process This stabilization, such as keep pH stable in 4.5-14.0 (preferably 5.5-13.0, more preferably 6.0-12.5, more preferably 7.0- 12.0, it is more preferably 8.0-11.0)；And/or
Wherein in step (4), keep the pH of suspension stable or base with alkali and acid respectively in the charging and reaction process This stabilization, such as keep pH stable in 4.5-12.0 (preferably 5.0-11.5, more preferably 6.0-11, more preferably 6.5- 10.0, it is more preferably 7.0-9.0).
8. according to the method described in claim 5, being wherein to use in the form of a solution for adjusting the acid of pH, the acid solution is Selected from one of hydrochloric acid solution, sulfuric acid solution, phosphoric acid solution or nitric acid solution or a variety of；And/or
It is wherein to use in the form of a solution for adjusting the alkali of pH, the aqueous slkali is selected from sodium hydroxide solution, hydroxide One of potassium solution, sodium carbonate liquor, solution of potassium carbonate, ammonia spirit are a variety of.
9. method according to claim 5 or 6, in which:
Titanium salt solution corresponding with titanium dioxide is by selected from TiCl4、Ti2(SO4)3And TiOSO4One of or a variety of titanium salts It is formed by solution；And/or
Magnesium salt solution corresponding with magnesia is by selected from MgSO4、MgCl2With Mg (NO3)2One of or a variety of titanium salts institute shape At solution；And/or
Silicate corresponding with silica or metasilicate solution are by selected from Na2SiO3、K2SiO3And MgSiO3In one Kind or a variety of salt are formed by solution.
10. according to the method described in claim 5, wherein drying be 80-180 DEG C (preferably 100-150 DEG C, more preferably 110-130 DEG C) at a temperature of dry -6 hours 1 hour, it is 3-5 hours more preferable；And/or
Wherein calcining is temperature lower calcination 5 minutes of 500 DEG C -900 DEG C (preferably 600-800 DEG C, 650-750 DEG C more preferable) ~30min, it is 10-15 minutes more preferable.
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