CN105036140B - Method for reducing viscosity of silicon dioxide slurry - Google Patents

Method for reducing viscosity of silicon dioxide slurry Download PDF

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Publication number
CN105036140B
CN105036140B CN201510369598.6A CN201510369598A CN105036140B CN 105036140 B CN105036140 B CN 105036140B CN 201510369598 A CN201510369598 A CN 201510369598A CN 105036140 B CN105036140 B CN 105036140B
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viscosity
silica slurry
silica
monomer
silicon dioxide
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CN105036140A (en
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王永庆
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Anhui Axi Green Technology Co.,Ltd.
Quecheng silicon Chemical Co., Ltd
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ANHUI QUECHENG SILICON CHEMICAL Co Ltd
Quechen Silicon Chemical Co Ltd
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Abstract

The invention provides a method for reducing the viscosity of silicon dioxide slurry, which comprises the steps of adding sodium metaaluminate into the silicon dioxide slurry, and the weight ratio of the sodium metaaluminate and silicon dioxide is 0.1 to 2 in a thousand; performing mechanical stirring, and then adding 0.1 to 3 in a thousand by weight of dispersant based on the silicon dioxide, performing the mechanical stirring again. According to the method for reducing the viscosity of the silicon dioxide slurry, the viscosity of the silicon dioxide slurry can be reduced under the condition that the solid contain is not reduced and the dosage of a viscosity reducing agent is reduced, the obtained silicon dioxide slurry has good mobility; the method for reducing the viscosity of the silicon dioxide slurry is conducive to the delivering of a pump and drying, and avoids the waste of water resources and the waste of energy sources.

Description

The method for reducing viscosity of silica slurry
Technical field
The present invention relates to the slurries of precipitated silica, and in particular to a kind of side of reduction viscosity of silica slurry Method.
Background technology
Precipitated silica, also known as white carbon, is used in many fields, for example rubber for tire manufacture, papermaking, paint, The fields such as feed addictive.
In traditional precipitated silica production technology, the silica slurry without treatment that drying is used, Its viscosity is high, poor fluidity, the low viscous purpose of drop is typically reached by the way of adding water, but also result in solid content simultaneously Reduction.Do not taken in traditional precipitated silica production procedure and effectively drop low viscous means.
Viscosity of silica slurry is high, poor fluidity, is not easy to pumping.Traditional using adds water to drop low viscous method Substantial amounts of water resource waste can be caused, needs to remove substantial amounts of water in high temperature drying, the waste of the energy is caused again.
CN101160261A discloses a kind of microparticulate silica, and it is adapted as making an addition to water or liquid tree In the liquid such as fat, coating, as tackifier used when carrying out the regulation of the viscoelastic properties such as its viscosity or thixotropy Enhancing-the filler of rheology modifier, silicon rubber or fluid sealant, CMP(Chemically mechanical polishing)Polishing agent, ink jet recording paper Surface smears.
CN101142287A is disclosed when a kind of pH when dispersion is 5-12 and is contained the two of partially hydrophobic silica Silica dispersion.
CN102286220A discloses a kind of preparation method of hydrophobic precipitated silicon dioxide, it is characterised in that comprising as follows Step:(1) dripped to coupling agent and polyethers are added dropwise in the poly- organic hydrogen-containing siloxane for adding acidic catalyst at 30~120 DEG C It is 0.5~3h between the added-time;(2) after completion of dropping, 0.5~5h is reacted at 80~150 DEG C, obtains final product surface modifier;(3) by surface Modifying agent is added in precipitated silica silicon original material, 0.5~5h of high speed shear under normal temperature;(4) the mixture pressure for obtaining (3) Filter, then dries 1~24h at 100~500 DEG C;(5) last size-reduced machine is crushed, and obtains final product hydrophobic precipitated silicon dioxide.
WO2004/018359A1 discloses a kind of aqueous dispersion containing SiO 2 powder, and wherein silica contains It is 10-60 weight % to measure, dispersion liquid stabilization in the range of the pH of 2-6, and the dispersion liquid, should also containing at least one compound In the aqueous solution that compound is at least partially soluble in the range of the pH of 2-6 in the form of the polyvalent cation, the cation is in class In silicic acid salt environment as SiO 2 powder particle surface anion component and stablize, the table of versus-silica Face, there is provided the amount of the compound of cation is compound/m that 0.001-0.1 mg provide cation2Silica surface, this is carried Compound for cation is calculated with oxide, and the current potential of the dispersion liquid has the value for being less than or equal to 0.
" stable mechanism of Ludox dispersed alumina slurry and exempt from degassing colloidal state consolidation in-situ forming prepare mullite ceramic Research ",《Chinese excellent MA theses full-text database engineering science and technology I volumes》, Kong Deyu on March 1st, 2005, discloses Aluminium chloride and when disclosing herein below pH=9.0, adds aluminium chloride steady for Ludox for the influence of Ludox Qualitative effect is extremely notable.However, what this text only studied is influence of the aluminium chloride to Ludox stability, stability and viscosity It is two entirely different concepts, such as stability is primarily referred to as preventing Ludox to be gelled.
The earlier patent application CN102718223A of the present inventor discloses a kind of side for reducing viscosity of silica slurry Sodium metaaluminate is added to silica slurry by method, the method according to aluminium ion and silica weight than the ratio for 0.5~5 ‰ In liquid, and by mechanical agitation, the method reduces the viscosity of slurry under conditions of slurry solid content is not reduced, resulting Silica slurry good fluidity, is conducive to the conveying and drying of pump, and this method also avoid water resource waste and The waste of the energy.However, the method is limited for the reduction of viscosity of silica slurry, and sodium metaaluminate is higher.By quoting The full content of the patent document is incorporated herein.
This area needs are a kind of can be with relatively low viscosity reducers(Such as sodium metaaluminate)Addition effectively reduces dioxy The method of SiClx slurry viscosity.
The content of the invention
The present inventor by further investigation and lot of experiments, there is provided it is a kind of can be with relatively low viscosity reducers usage amount The method for effectively to reduce viscosity of silica slurry, and the solid content of slurries is not reduced.
A kind of method for reducing viscosity of silica slurry, the method is by sodium metaaluminate according to aluminium ion than silica weight Amount is added in silica slurry than the ratio for 0.1~2 ‰, and by mechanical agitation, is then added based on titanium dioxide The dispersant of silicon weight meter 0.1~3 ‰, then carry out mechanical agitation.
The time stirred for the first time is preferably 1-3h, and the time of second stirring is preferably 0.5-2h.
The dispersant is preferably obtained by making following monomer mixture copolymerization, and the monomer mixture includes following monomer Or by following monomer composition:(a) 70-95mol% methacrylic acid monomers;(b) 3-15mol% ethylenically unsaturated carboxylic acids or its acid Acid anhydride;Monomer shown in (c) 1-10mol% following formula Is;Monomer shown in (d) 0.2-5mol% Formula Ils:
Formula(I)
Formula(II)
Wherein, n is the integer of 4-8, preferably 3-5, R1And R2It is independently of one another C1-C4 straight or branched alkyls, preferably It is C1-C3 alkyl, more preferably methyl or ethyl.
The ethylenically unsaturated carboxylic acids or its acid anhydrides are preferably such as itaconic acid, fumaric acid, maleic acid, itaconic anhydride, horse Carry out acid anhydrides etc..
Herein it should be noted that such dispersant of the invention is there is not yet report, nor the conventional selection of this area, But those skilled in the art are by a large amount of further investigation exploitations.
The inventors discovered that, the dispersant can make silica slurry keep in higher concentrations good mobility and Stability, so that with good aid pumpability.Primary Study shows, in the case of identical mobility, the dispersant Addition can make silica solid content improve about 5-15 weight %.On its viscosity-reducing mechanism, show after further study, this point Powder can form certain hydrophobic structure in silica surface, more importantly, can make silica dispersion have compared with Low isoelectric point, it is to avoid the adhesion between silica dioxide granule.
The preparation of the dispersant can be carried out by the typical polymerization methods of this area.
Polymerization can be carried out using the conventional polymerization in this area, such as polymerisation in bulk, polymerisation in solution, emulsion Polymerization or suspension polymerisation.The formula(I)With(II)Compound can for example be purchased from Fluka companies with commercially available, It is referred to the acquisition of low-polyacrylate synthetic method.
Wherein, in the sodium metaaluminate weight of the addition aluminium ion weight can be silica slurry weight 0.1~ 1‰。
The solid content of the silica slurry can be 20~30%.
The sodium metaaluminate can be pure sodium metaaluminate solid, or can be reacted by aluminium hydroxide and NaOH The aqueous solution for obtaining.When using aqueous solution form, its addition in silica slurry is still based on sodium metaaluminate weight Meter.
The sodium metaaluminate aqueous solution can be that aluminium hydroxide mixes with NaOH by weight proportion 1~2.5: 1, then add The water for entering the 30~70% of mixture weight boils and obtains.
The sodium metaaluminate aqueous solution can be that aluminium hydroxide mixes with NaOH by weight proportion 2: 1, add mixed The water of the 60% of polymer weight boils and obtains.
The mass concentration for boiling the sodium metaaluminate aqueous solution for obtaining can be 30%~50%.
The sodium metaaluminate aqueous solution can be that aluminium hydroxide mixes with caustic soda, add water to boil, after then boiling The product filtering arrived, takes what supernatant was obtained.
In an especially preferred embodiment, the sodium metaaluminate be prepared via a method which to obtain it is modified partially Sodium aluminate:
(1)Sodium hydroxide solution is prepared, the ratio between the quality of NaOH and the volume of deionized water are 200-1000:1(g/ L);
(2)To step(1)Aluminium hydroxide is added in the sodium hydroxide solution, 4-6 is reacted at 140 DEG C -155 DEG C small When, activated carbon is added, sodium aluminate solution is obtained after filtering, cooling, add based on the steady of sodium metaaluminate weight meter 0.1-0.3% Determine agent, obtain final products sodium aluminate solution, the concentration of the sodium aluminate solution is calculated as 260-300g/ with alundum (Al2O3) L, the stabilizer is kayexalate.
In an especially preferred embodiment, the aluminum oxide is bayerite form.Research discovery, uses three hydroxyls The aluminum oxide of aluminium stone form, compared to the aluminum oxide such as α-Al of other forms2O3Or boehmite, can make obtained inclined More than one times of impurity content reduction in sodium aluminate.This special-effect of the bayerite in silica viscosity reduction is in existing skill There is not yet report in art.
It is moreover found that kayexalate is compared to other common stabilizer such as triethanolamines, can be more effective Suppress the generation that sodium metaaluminate places facile hydrolysis, sedimentation problem for a long time, such as when using kayexalate, hydrolyzing Preceding effective storage period is more than 2 times when using triethanolamine.Additionally, the consumption of kayexalate is than triethanolamine It is few a lot, reduce the introducing of undesirable material.
In another preferred embodiment of the invention, the need for product specification can also being regarded, to silica slurry Sodium metaphosphate and sodium lignin sulfonate 1 are added in liquid:3~3:1 weight than mixture.The addition of the mixture is based on dioxy SiClx weight is calculated as 0.1~0.5 ‰.The mixture can play further peptizaiton to silica, so that further Reduce the viscosity of silica slurry.
On the other hand, there is provided the silica slurry, the viscosity of the silica slurry can for 150~ 800cP (centipoise), preferably 150-500 cP (centipoise), most preferably from about 150P (centipoise).
On the other hand, there is provided the silica slurry is preparing rubber for tire, papermaking, preparing paint and prepare and raise Application in feed additives.
It yet still another aspect, there is provided can be used for reduce viscosity of silica slurry dispersant, the dispersant by make as Lower monomer mixture copolymerization is obtained, and the monomer mixture includes following monomer or by following monomer composition:(a)70-95mol% Methacrylic acid monomer;(b) 3-15mol% ethylenically unsaturated carboxylic acids or its acid anhydrides;List shown in (c) 1-10mol% following formula Is Body;Monomer shown in (d) 0.2-5mol% Formula Ils:
Formula(I)
Formula(II)
Wherein, n is the integer of 3-8, preferably 3-5, R1And R2It is independently of one another C1-C4 straight or branched alkyls, preferably It is C1-C3 straight chained alkyls, more preferably ethyl.
Described ethylenically unsaturated carboxylic acids or derivatives thereof are preferably such as itaconic acid, fumaric acid, maleic acid, itaconic anhydride, Maleic anhydride etc..
Low viscous method drops in the silica slurry that the present invention is provided, and is not reducing slurry solid content and viscosity reducers Under conditions of consumption is reduced, the viscosity of slurry, the silica slurry good fluidity of gained, so as to be conducive to the conveying of pump are reduced And dry, and this method also avoid the waste of water resource and the waste of the energy.
Specific embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
Embodiment 1
The preparation of dispersant:
By following monomer mixture copolymerization, the monomer mixture is by following monomer composition:(a) 85mol% methacrylic acids Monomer;(b) 8mol% itaconic acid acid anhydrides;Monomer shown in (c) 5mol% following formula Is;Monomer shown in (d) 2mol% Formula Ils:
Formula(I)
Formula(II)
Wherein, n is 4, R1And R2It is methyl,
Using emulsion polymerization, mix to monomer described in 80g is added in round-bottomed flasks of the 500mL with mechanical stirring device Thing and 200mL deionized waters, logical nitrogen under stirring are subsequently adding 0.1g ammonium persulfates as initiator, are warming up to polymerization temperature Degree, polymerization temperature is 80 DEG C, keeps reaction 3 hours, and polymerizate is reclaimed after terminating reaction.
Embodiment 2
By the sodium metaaluminate aqueous solution that 3g mass concentrations are 50% and the silica slurry that 10kg viscosity is 8000cP, two The solid content of silica slurry is 24.2%, is added in the reactor with agitating device, is stirred, and is subsequently adding 1.5g The dispersant that embodiment 1 is obtained, then be stirred to uniform, testing size, gained slurries silica viscosity is 600cP(Cloth Family name's viscosimeter, tests under normal temperature), solid content is 24.2%.Solid content is institute of the solid gross mass divided by composition slurries in slurries What the quality for having component was obtained.
Comparative example 1
The comparative example is the embodiment in CN102718223A.By the sodium metaaluminate aqueous solution that 10g mass concentrations are 50% It is the silica slurry of 8000cP with 10kg viscosity, the solid content of silica slurry is 24.2%, is added to stirring In the reactor of device, testing size after stirring, gained slurries silica viscosity is 900cP(Brookfield viscometer, normal temperature Lower test), solid content is 24.2%.Solid content is that solid gross mass is obtained divided by the quality of all components of composition slurries in slurries Arrive.
Clearly be can be seen that when using dispersant of the invention, not only by the result of above-described embodiment and comparative example Can reduce the consumption of sodium metaaluminate, but also the slurries silica viscosity is reduced by a larger margin, it reduces journey Du Dayue 33%.It is such to have the technical effect that what those skilled in the art to be expected.
This written description discloses the present invention, including optimal mode using example, and also enables those skilled in the art Manufacture and use the present invention.It is of the invention can patentable scope be defined by the claims, and this area skill can be included Other examples that art personnel expect.If this other examples have the structural elements of literal language not different from claims Element, or if this other examples include equivalent structure element of the literal language without substantial differences with claims, Then this other examples are intended within the scope of claims.In the case where inconsistent degree is not resulted in, by reference to The all references part of reference herein is incorporated herein.

Claims (6)

1. a kind of method for reducing viscosity of silica slurry, the method comprises the following steps:By sodium metaaluminate according to aluminium ion It is added in silica slurry than the ratio for 0.1~2 ‰ than silica weight, and by mechanical agitation, is then added again Enter the dispersant based on silica weight 0.1~3 ‰, then carry out mechanical agitation;
The dispersant is obtained by making following monomer mixture copolymerization, and the monomer mixture includes following monomer or by as follows Monomer composition:(a) 70-95mol% methacrylic acid monomers;(b) 3-15mol% ethylenically unsaturated carboxylic acids or its acid anhydrides;(c) Monomer shown in 1-10mol% following formula Is;Monomer shown in (d) 0.2-5mol% Formula Ils:
Wherein, n is the integer of 4-8, R1And R2It is independently of one another C1-C4 straight or branched alkyls.
2. it is according to claim 1 reduce viscosity of silica slurry method, it is characterised in that the silica slurry The solid content of liquid is 25~35%.
3. the method for reducing viscosity of silica slurry according to claim 1, it is characterised in that the sodium metaaluminate is Pure sodium metaaluminate solid, or the aqueous solution for obtaining is reacted by aluminium hydroxide and NaOH.
4. the silica slurry for being obtained according to any described method of claims 1 to 3, it is characterised in that the viscosity of slurries It is 150~800cP.
5. the silica slurry described in claim 4 is preparing rubber for tire, papermaking, preparing paint and is preparing feed addictive In application.
6. it is a kind of can be used for reduce viscosity of silica slurry dispersant, the dispersant is by making following monomer mixture copolymerization Obtain, the monomer mixture includes following monomer or by following monomer composition:(a) 70-95mol% methacrylic acid monomers; (b) 3-15mol% ethylenically unsaturated carboxylic acids or its acid anhydrides;Monomer shown in (c) 1-10mol% following formula Is;(d) 0.2-5mol% Monomer shown in Formula Il:
Wherein, n is the integer of 3-8, R1And R2It is independently of one another C1-C4 straight or branched alkyls.
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CN107151350B (en) * 2017-04-24 2019-06-07 确成硅化学股份有限公司 A kind of preparation method of high fluidity silica
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CN114085566A (en) * 2021-12-07 2022-02-25 安徽进化硅纳米材料科技有限公司 Aqueous silicon dioxide suspension, preparation method and application thereof

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JP5906635B2 (en) * 2011-09-26 2016-04-20 富士ゼロックス株式会社 Method for producing silica particle dispersion
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Address after: Fengqiao Industrial Park, Chuyang City, Anhui Province

Patentee after: Anhui Axi Green Technology Co.,Ltd.

Patentee after: Quecheng silicon Chemical Co., Ltd

Address before: Fengqiao Industrial Park, Chuyang City, Anhui Province

Patentee before: ANHUI QUECHEN SILICON CHEMICAL CO.,LTD.

Patentee before: Quecheng silicon Chemical Co., Ltd