CN108793250A - A kind of preparation method of low viscosity antimony pentoxide hydrosol - Google Patents
A kind of preparation method of low viscosity antimony pentoxide hydrosol Download PDFInfo
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- C01—INORGANIC CHEMISTRY
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- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
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Abstract
A kind of preparation method of low viscosity antimony pentoxide hydrosol, includes the following steps：（1）After water is heated, antimony oxide is added and is mixed, heating stirring is continued, hydrogen peroxide is added and is reacted；（2）Concentration, and in concentration process, stabilizer is added in substep, after concentration, cools down immediately, then adjust pH value, obtains low viscosity antimony pentoxide hydrosol.The method of the present invention stabilizing agent dosage is few, and prepared low viscosity antimony pentoxide hydrosol appearance is limpid milky, yellowish, glossy, good fluidity, wherein the mass content of antimony pentoxide is 48~54%, and pH value is 6.1~6.8, viscosity（25℃）< 15mPas, proportion（Room temperature）Be 1.751~1.849, stability is preferable, antimony pentoxide by the hydrosol to organosol direct yield >=98.5%；The method of the present invention preparation process is simple, easy to operate, at low cost, environmentally protective.
Description
Technical field
The present invention relates to a kind of preparation methods of antimony pentoxide hydrosol, and in particular to a kind of low viscosity antimony pentoxide
The preparation method of the hydrosol.
Background technology
Antimony is as national strategy goods and materials, dosage picture industry monosodium glutamate, but is allusion quotation again with non-renewable after antimony product use
The scarce resource of type converts antimony to the utilization rate that antimony will be improved after antimony pentoxide hydrosol.Antimony pentoxide hydrosol master
It is used for that fabric, coating, non-woven fabrics, adhesive, fiber and other material to make fire retarding synergist and petrochemical industry makees passivator, dispersion
It is small to spend height, good fluidity, grain size.
The general preparation method of antimony pentoxide hydrosol is that oxidant is added（Such as H2O2）, antimony oxide is made to be oxidized to
Antimony pentoxide, the antimony pentoxide for aoxidizing generation form 0.03 μm or so of particle, but since antimony pentoxide hydrosol is
The polymolecular aggregation of insoluble substance is formed by dispersion in the medium, and there are sizable boundaries between particle and medium
Face.From thermodynamic significance, this system is not real stabilising system, due to larger interface, it is meant that body
System has sizable surface energy, thus is easy interaction and generates coagulation phenomenon, bad dispersibility.Therefore, in no stabilizer
Under the action of, the antimony pentoxide hydrosol that simple oxidation generates is unstable, and standing will generate precipitation too long, be not
Energy long-term preservation, the serious normal use for affecting antimony pentoxide hydrosol.
The antimony pentoxide hydrosol product of existing company's production is divided into 30 glue and 50 glue according to the content of antimony pentoxide,
Stabilizer used is alkanolamine, although their effects between hydrone are very strong, stability is good, and it is viscous to easily cause product
Spend height.30% or so, stabilizer is put into the antimony pentoxide content of 30 glue before oxidation, and transparency is high, good fluidity, is glued
Degree（25℃）< 5mPas, and the antimony pentoxide content of 50 glue, 50% or so, concentration is bigger, and viscosity is higher.Therefore, it obtains
A kind of this high concentration of 50 glue is obtained, but the preparation method of the low antimony pentoxide hydrosol of viscosity is technology urgently to be resolved hurrily simultaneously
Problem.
CN1074945A discloses a kind of preparation of colloidal antimony pentoxide by chlorination hydrolysis process, is to use SbCl5Solution with 3~
10 times of water are hydrolyzed, and still, liquid has a large amount of chlorine-contained wastewater disposition after hydrolysis.
CN1978312A discloses a kind of inorganic oxide sol being modified using high molecular compound stabilizer and its system
Preparation Method is with the one or more in macromolecular compound polyvinyl alcohol, polyethylene glycol, polyoxyethylene, polystyrene
Mixture is prepared for the good aluminium oxide of stability, zirconium oxide, silica, calcium oxide, antimony pentoxide, two as stabilizer
One or more kinds of inorganic oxide sols in cerium oxide, yttrium oxide, zinc oxide, nickel oxide, chromium oxide, titanium oxide.
But dilute glue that this method products therefrom is a kind of stability, it is not directed to the viscosity problem of dense glue after concentration.
CN101024515A discloses a kind of production new technique of colloidal antimony pentoxide, is to be added to stablize before oxidation
Agent generates dilute glue, and for dilute glue before not concentrating, viscosity is generally all very low, then colloid dry powder is made with spray drying process.Dilute glue one
As will not plug nozzle, but because in dilute glue antimony pentoxide content be less than 20%, this method to improve 50% colloid viscosity have no
Directive significance.
CN101327954A discloses a kind of antimony pentoxide fluid dispersion and preparation method, five oxidations two of this method production
Antimony dispersion liquid is by antimony oxide, organic acid, dispersion stabilizer, water and hydrogen peroxide by weight 1:2~2.5%:2~
5%:3~5:2~5 hybrid reactions form, and wherein content of hydrogen peroxide is 50%.But due to the actual amount phase of hydrogen peroxide
For the theoretical weight ratio 1 of antimony oxide and hydroperoxidation:0.47, excessive very much, therefore, solution is in acidity, easily
Etching apparatus.
104355333 A of CN disclose a kind of preparation method of antimony pentoxide composite dry powder, are that raw material three is aoxidized two
Antimony is dissolved in concentrated hydrochloric acid, and the weight ratio of the concentrated hydrochloric acid and antimony oxide is 12~13:1, controlled at 80 DEG C.But
The defect of this method is that concentrated hydrochloric acid is volatility strong acid, not only can etching apparatus, but also cause severe operational environment.
CN101798112A discloses a kind of method preparing antimony pentoxide hydrosol and its dry powder with compound stabilizer,
The compound stabilizer is triethanolamine and phosphoric acid is formed by triethanolamine phosphate solution, and product is five oxygen of 40% concentration
Change the two antimony hydrosols.Stabilizer used in this method is triethanolamine, its effect between hydrone is very strong, and product viscosity is high；Phosphorus
Acid hydroxyl containing there are three, also will increase dispersion viscosity.But products obtained therefrom is confined to 40% concentration and five oxidation below
The two antimony hydrosols, and the antimony pentoxide hydrosol viscosity for being further condensed into 50% concentration can be higher.
Invention content
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide a kind of gained five
Aoxidize that the water-soluble adhesiveness of two antimony is low, and stability is good, easy to use, simple for process, easy to operation, at low cost, environmentally protective is low
The preparation method of viscosity antimony pentoxide hydrosol.
The technical solution adopted by the present invention to solve the technical problems is as follows：A kind of low viscosity antimony pentoxide hydrosol
Preparation method includes the following steps：
（1）After water is heated, antimony oxide is added and is mixed, the antimony oxide hydrosol is obtained, continues heating stirring, is added
Hydrogen peroxide is reacted, and water-soluble antimony pentoxide sol is obtained；
（2）By step（1）Gained water solubility antimony pentoxide sol is concentrated, and in concentration process, and substep, which is added, to be stablized
Agent after concentration, cools down, then adjusts pH value immediately, obtains low viscosity antimony pentoxide hydrosol.
Preferably, step（1）In, when water temperature >=50 DEG C, antimony oxide is added and is mixed.Antimony oxide particle
Be more easy under the water temperature it is evenly dispersed in water.
Preferably, step（1）In, when temperature >=65 DEG C of the antimony oxide hydrosol, stops heating, add dioxygen
Water is reacted.It is exothermic process that reaction, which is added, in hydrogen peroxide, and the temperature of aqueous solution will continue to rise.
Preferably, step（1）In, the addition speed of the hydrogen peroxide is 2~4L/min.If the addition speed of hydrogen peroxide is too
Slowly, then reaction time consumption is long, and production cost increases, if the addition speed of hydrogen peroxide is too fast, reaction is violent, is easy to emit slot.
Preferably, step（1）In, the mass volume ratio of the antimony oxide and water（kg/L）It is 1:5~7（More preferably
1:5.5~6.5）.
Preferably, step（1）In, the molar ratio of the antimony oxide and hydrogen peroxide in hydrogen peroxide is 1:2.0~
2.5.Under the molar ratio, raw material antimony oxide can be fully oxidized complete.
Preferably, step（1）In, the mass concentration of the hydrogen peroxide is 26.0~35.0%.
Preferably, step（1）In, the temperature of the reaction is 50~90 DEG C, and the time of reaction is 3~5h.Due to dioxygen
The addition of water is exothermic process, and after temperature is more than 90 DEG C, solution meeting vigorous reaction is easy to emit slot.When reaction temperature is more than 90
DEG C when, cooling water cooling can be used, to ensure that reaction temperature is no more than 90 DEG C.
Preferably, step（2）In, the temperature of the concentration is 100 DEG C, and it is 1.700~1.750 to be to be concentrated into colloidal sol proportion
Only.
Preferably, step（2）In, the dosage of the stabilizer is the 7.0~10.0% of raw material antimony oxide quality.If
The dosage of stabilizer is very few, then antimony pentoxide cohesion is not thorough, and antimony pentoxide is caused to lose, if stabilizing agent dosage is excessive,
Antimony pentoxide viscosity can then increased, cost increases.After forming water-soluble antimony pentoxide sol, it is suitably steady that dosage is added
Determine agent, advantageously reduces the viscosity of Diantimony Pentoxide Colloid.
Preferably, step（2）In, the stabilizer is triethanolamine.The stabilizer is alkanolamine, and polarity is strong, with
Active force between hydrone is big, and the stabilizer is different from the existing hydrosol using phosphoric acid as stabilizer used, with
The viscosity of the increase of stabilizer addition, Diantimony Pentoxide Colloid can also increase therewith.In the method for the present invention, stabilizer plays steady
Tailor-made mode is：Stablize agent molecule colloidal solid is all wrapped up in colloidal dispersion medium, make it not with it is other
Colloidal solid contacts, and the high surface energy of colloidal grain surface cannot display, to improve the stability of colloidal solid.
Preferably, step（2）In, it is that stabilizer is divided into >=4 additions that stabilizer, which is added, in the substep.
Preferably, step（2）In, the concrete operations that stabilizer is added in the substep are：When colloidal sol proportion reaches 1.240~
When 1.300, the stabilizer for being equivalent to raw material antimony oxide quality 2.00~2.60% is added, is stirred to react；When colloidal sol proportion reaches
When to 1.400~1.450, the stabilizer for being equivalent to raw material antimony oxide quality 0.80~1.30% is added, is stirred to react；When
When colloidal sol proportion reaches 1.500~1.550, the stabilizer for being equivalent to raw material antimony oxide quality 1.00~1.60% is added, stirs
Mix reaction；When colloidal sol proportion reaches 1.600~1.650, addition is equivalent to raw material antimony oxide quality 1.00~1.70%
Stabilizer is stirred to react；When colloidal sol proportion reaches 1.700~1.750, addition is equivalent to raw material antimony oxide quality 2.20
~2.80% stabilizer, is stirred to react.The present inventor, which studies, to be found：（1）Stabilizer is added after the generation of antimony pentoxide molecule
It is got well than being added in antimony oxide oxidation process, because stabilizer is added in oxidation process, antimony pentoxide molecule exists
In generating process with stablize agent molecule formed chemical bond, so that this Diantimony Pentoxide Colloid molecule is stable in the presence of in water, need
It wants the stabilization agent molecule of 0.8~1.0mol to be combined with 1mol antimony pentoxide molecules and can be only achieved stabilization, the dosage of stabilizer is special
It is not big；And stabilizer is added after antimony pentoxide generates, to form stable antimony pentoxide hydrosol, 6~7mol
Antimony pentoxide molecule only needs to be combined with 1mol stabilization agent molecules, this is because generating a period of time in antimony pentoxide molecule
Afterwards, they, which are mutually gathered into, compares bulky grain, that is to say, that and it is mostly many containing antimony pentoxide molecule in particle at this moment,
Stablize agent molecule also just corresponding reduction needed for these particles for wrapping up；（2）In the Diantimony Pentoxide Colloid of same concentrations,
Stabilizer is added in oxidation process or after the completion of oxidation, the viscosity difference for being formed by stable colloid is larger, in oxidation process
Be added stabilizer formed colloid, viscosity can much higher, and viscosity is excessive, product poor fluidity, poor dispersion, easily agglomerate or
Gel；And after the completion of aoxidizing, in concentration process, when colloidal sol proportion reaches 1.240~1.300, addition is equivalent to raw material three
The stabilizer of two antimony quality 2.00~2.60% is aoxidized, if stabilizer is added too late, solution if is difficult to plastic, when colloidal sol proportion
When reaching 1.400~1.450, the stabilizer for being equivalent to raw material antimony oxide quality 0.80~1.30% is added, when colloidal sol proportion
When reaching 1.500~1.550, the stabilizer for being equivalent to raw material antimony oxide quality 1.00~1.60% is added, substep is added steady
Determine agent, solution is made gradually to start plastic, when colloidal sol proportion reaches 1.600~1.650, addition is equivalent to raw material antimony oxide
The stabilizer of quality 1.00~1.70%, when colloidal sol proportion reaches 1.700~1.750, is added at this point, solution has generated colloidal sol
It is equivalent to the stabilizer of raw material antimony oxide quality 2.20~2.80%, the time of stabilizer concentration is reduced, advantageously reduces molten
The viscosity of glue.
Preferably, step（2）In, the cooling immediately refers to being cooled to≤60 DEG C in 20~30min.After cooling
The proportion when proportion of products obtained therefrom can be finished compared with concentration is high.
Preferably, step（2）In, pH value is adjusted to 6.1~6.8 with alkaline matter（More preferable 6.4~6.6）.It is water-soluble
The pH value of antimony pentoxide sol, in the case of no stabilizer, generally 1~2；After stabilizer is added, generally 4~6,
Production medium is faintly acid, and by adjusting pH value to 6.1~6.8, when use will not cause corrosivity to equipment pipe, to equipment
Also without particular/special requirement.
Preferably, step（2）In, the alkaline matter is triethanolamine, one kind in diethanol amine or monoethanolamine etc.
Or it is several（More preferable monoethanolamine）.
The method of the present invention has the beneficial effect that：
（1）The method of the present invention stabilizing agent dosage is few, and prepared low viscosity antimony pentoxide hydrosol appearance is limpid milky white
Color, yellowish, glossy, good fluidity, wherein the mass content of antimony pentoxide is 48~54 %, the matter of antimony oxide
Content≤0.41% is measured, pH value is 6.1~6.8, viscosity（25℃）< 15mPas, proportion（Room temperature）It is 1.741~1.849, puts
It sets half a year, antimony pentoxide can be evenly dispersed in organic phase, sedimentation of not reuniting；Antimony pentoxide is by the hydrosol to organosol
Direct yield >=98.5%；Since the dissolubility and stability of the low viscosity antimony pentoxide hydrosol of the method for the present invention preparation are non-
Chang Hao convenient for packaging, transport and uses, makees fire retarding synergist especially suitable for fabric, coating, non-woven fabrics, adhesive, fiber etc.
And petrochemical industry makees passivator use；
（2）The method of the present invention preparation process is simple, easy to operate, at low cost, and three wastes generate, environmentally protective.
Specific implementation mode
With reference to embodiment, the invention will be further described.
The mass concentration of hydrogen peroxide used in the embodiment of the present invention is 27.5%, density 1.13g/mL；The present invention is implemented
Raw material or chemical reagent are obtained by routine business approach unless otherwise specified used in example.
Embodiment 1
（1）After 2500L water is heated to 50 DEG C, 400kg is added（1372mol）Antimony oxide is mixed, and three oxidations two are obtained
The antimony hydrosol when temperature of continuation heating stirring to the antimony oxide hydrosol is 70 DEG C, stops heating, then with speed 3L/min
310L is added（Hydrogen peroxide 2833mol）Hydrogen peroxide carry out reaction 3h at 80 DEG C, obtain water-soluble antimony pentoxide sol
（Proportion 1.113）；
（2）By step（1）For gained water solubility antimony pentoxide sol at 100 DEG C, it is 1.715 to be concentrated into colloidal sol proportion
Only, and in concentration process, triethanolamine is added in substep, after concentration, in 25min, is cooled to 60 DEG C immediately, then with one
Ethanol amine adjusts pH value to 6.5, obtains 815kg low viscosity antimony pentoxide hydrosols；The specific of triethanolamine is added in the substep
Operation is：When colloidal sol proportion reaches 1.240,10kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.420,
5kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.600,6kg triethanolamines are added, are stirred to react；When molten
When glue proportion reaches 1.710,11kg triethanolamines are added, are stirred to react.
Low viscosity antimony pentoxide hydrosol appearance prepared by the embodiment of the present invention is limpid milky, yellowish,
It is glossy, good fluidity, wherein the mass content of antimony pentoxide is 48.50%, and the mass content of antimony oxide is
0.33%, pH value 6.5, viscosity（25℃）For 8.0mPas, proportion（Room temperature）It is 1.751, places half a year, antimony pentoxide energy
It is evenly dispersed in organic phase, sedimentation of not reuniting；Antimony pentoxide is 98.99% by the direct yield of the hydrosol to organosol；Work
Three wastes generate during skill.
Embodiment 2
（1）After 4500L water is heated to 52 DEG C, 750kg is added（2573mol）Antimony oxide is mixed, and three oxidations two are obtained
The antimony hydrosol when temperature of continuation heating stirring to the antimony oxide hydrosol is 75 DEG C, stops heating, then with speed 2L/min
616L is added（Hydrogen peroxide 5628mol）Hydrogen peroxide carry out reaction 3.5h at 85 DEG C, it is molten to obtain water-soluble antimony pentoxide
Glue（Proportion 1.115）；
（2）By step（1）For gained water solubility antimony pentoxide sol at 100 DEG C, it is 1.740 to be concentrated into colloidal sol proportion
Only, and in concentration process, triethanolamine is added in substep, after concentration, in 20min, is cooled to 60 DEG C immediately, then with one
Ethanol amine adjusts pH value to 6.4, obtains 1455kg low viscosity antimony pentoxide hydrosols；The specific of triethanolamine is added in the substep
Operation is：When colloidal sol proportion reaches 1.290,19.5kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.440
When, 9.5kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.520,11kg triethanolamines are added, stirring is anti-
It answers；When colloidal sol proportion reaches 1.630,9kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.735, it is added
18kg triethanolamines, are stirred to react.
Low viscosity antimony pentoxide hydrosol appearance prepared by the embodiment of the present invention is limpid milky, yellowish,
It is glossy, good fluidity, wherein the mass content of antimony pentoxide is 53.66%, and the mass content of antimony oxide is
0.31%, pH value 6.4, viscosity（25℃）For 7.0mPas, proportion（Room temperature）It is 1.830, places half a year, antimony pentoxide energy
It is evenly dispersed in organic phase, sedimentation of not reuniting；Antimony pentoxide is 98.60% by the direct yield of the hydrosol to organosol；Work
Three wastes generate during skill.
Embodiment 3
（1）After 4400L water is heated to 53 DEG C, 800kg is added（2744mol）Antimony oxide is mixed, and three oxidations two are obtained
The antimony hydrosol when temperature of continuation heating stirring to the antimony oxide hydrosol is 69 DEG C, stops heating, then with speed 3L/min
720L is added（Hydrogen peroxide 6580mol）Hydrogen peroxide carry out reaction 4h at 70 DEG C, obtain water-soluble antimony pentoxide sol
（Proportion 1.091）；
（2）By step（1）For gained water solubility antimony pentoxide sol at 100 DEG C, it is 1.750 to be concentrated into colloidal sol proportion
Only, and in concentration process, triethanolamine is added in substep, after concentration, in 25min, is cooled to 55 DEG C immediately, then with two
Ethanol amine adjusts pH value to 6.6, obtains 1530kg low viscosity antimony pentoxide hydrosols；The specific of triethanolamine is added in the substep
Operation is：When colloidal sol proportion reaches 1.275,17kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.420,
9kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.530,8kg triethanolamines are added, are stirred to react；When molten
When glue proportion reaches 1.620,8kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.720, tri- second of 18kg is added
Hydramine is stirred to react.
Low viscosity antimony pentoxide hydrosol appearance prepared by the embodiment of the present invention is limpid milky, yellowish,
It is glossy, good fluidity, wherein the mass content of antimony pentoxide is 51.80%, and the mass content of antimony oxide is
0.41%, pH value 6.6, viscosity（25℃）For 10.0mPas, proportion（Room temperature）It is 1.810, places half a year, antimony pentoxide
Can be evenly dispersed in organic phase, sedimentation of not reuniting；Antimony pentoxide is 98.50% by the direct yield of the hydrosol to organosol；
Three wastes generate in technical process.
Embodiment 4
（1）After 5500L water is heated to 50 DEG C, 850kg is added（2916mol）Antimony oxide is mixed, and three oxidations two are obtained
The antimony hydrosol when temperature of continuation heating stirring to the antimony oxide hydrosol is 68 DEG C, stops heating, then with speed 4L/min
649L is added（Hydrogen peroxide 5932mol）Hydrogen peroxide carry out reaction 4.5h at 75 DEG C, it is molten to obtain water-soluble antimony pentoxide
Glue（Proportion 1.113）；
（2）By step（1）For gained water solubility antimony pentoxide sol at 100 DEG C, it is 1.740 to be concentrated into colloidal sol proportion
Only, and in concentration process, triethanolamine is added in substep, after concentration, in 30min, is cooled to 50 DEG C immediately, then with one
Ethanol amine adjusts pH value to 6.5, obtains 1640kg low viscosity antimony pentoxide hydrosols；The specific of triethanolamine is added in the substep
Operation is：When colloidal sol proportion reaches 1.270,20kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.410,
8.5kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.510,10kg triethanolamines are added, are stirred to react；When
When colloidal sol proportion reaches 1.625,12kg triethanolamines are added, are stirred to react；When colloidal sol proportion reaches 1.715,22kg is added
Triethanolamine is stirred to react.
Low viscosity antimony pentoxide hydrosol appearance prepared by the embodiment of the present invention is limpid milky, yellowish,
It is glossy, good fluidity, wherein the mass content of antimony pentoxide is 51.38%, and the mass content of antimony oxide is
0.40%, pH value 6.5, viscosity（25℃）For 9.0mPas, proportion（Room temperature）It is 1.805, places half a year, antimony pentoxide energy
It is evenly dispersed in organic phase, sedimentation of not reuniting；Antimony pentoxide is 98.59% by the direct yield of the hydrosol to organosol；Work
Three wastes generate during skill.
Claims (9)
1. a kind of preparation method of low viscosity antimony pentoxide hydrosol, which is characterized in that include the following steps：
（1）After water is heated, antimony oxide is added and is mixed, the antimony oxide hydrosol is obtained, continues heating stirring, is added
Hydrogen peroxide is reacted, and water-soluble antimony pentoxide sol is obtained；
（2）By step（1）Gained water solubility antimony pentoxide sol is concentrated, and in concentration process, and substep, which is added, to be stablized
Agent after concentration, cools down, then adjusts pH value immediately, obtains low viscosity antimony pentoxide hydrosol.
2. the preparation method of low viscosity antimony pentoxide hydrosol according to claim 1, it is characterised in that：Step（1）In,
When water temperature >=50 DEG C, antimony oxide is added and is mixed；When temperature >=65 DEG C of the antimony oxide hydrosol, stop adding
Heat adds hydrogen peroxide and is reacted；The addition speed of the hydrogen peroxide is 2~4L/min.
3. the preparation method of low viscosity antimony pentoxide hydrosol according to claim 1 or claim 2, it is characterised in that：Step（1）
In, the mass volume ratio of the antimony oxide and water is 1:5~7；The antimony oxide and hydrogen peroxide in hydrogen peroxide
Molar ratio is 1:2.0~2.5；The mass concentration of the hydrogen peroxide is 26.0~35.0%.
4. according to the preparation method of one of claims 1 to 3 low viscosity antimony pentoxide hydrosol, it is characterised in that：Step
Suddenly（1）In, the temperature of the reaction is 50~90 DEG C, and the time of reaction is 3~5h.
5. according to the preparation method of one of Claims 1 to 4 low viscosity antimony pentoxide hydrosol, it is characterised in that：Step
Suddenly（2）In, the temperature of the concentration is 100 DEG C, is concentrated into until colloidal sol proportion is 1.700~1.750.
6. according to the preparation method of one of Claims 1 to 5 low viscosity antimony pentoxide hydrosol, it is characterised in that：Step
Suddenly（2）In, the dosage of the stabilizer is the 7.0~10.0% of raw material antimony oxide quality；The stabilizer is three ethyl alcohol
Amine.
7. according to the preparation method of one of claim 1~6 low viscosity antimony pentoxide hydrosol, it is characterised in that：Step
Suddenly（2）In, it is that stabilizer is divided into >=4 additions that stabilizer, which is added, in the substep；The specific behaviour of stabilizer is added in the substep
As：When colloidal sol proportion reaches 1.240~1.300, addition is equivalent to the steady of raw material antimony oxide quality 2.00~2.60%
Determine agent, is stirred to react；When colloidal sol proportion reaches 1.400~1.450, addition be equivalent to raw material antimony oxide quality 0.80~
1.30% stabilizer, is stirred to react；When colloidal sol proportion reaches 1.500~1.550, addition is equivalent to raw material antimony oxide
The stabilizer of quality 1.00~1.60%, is stirred to react；When colloidal sol proportion reaches 1.600~1.650, addition is equivalent to raw material
The stabilizer of antimony oxide quality 1.00~1.70%, is stirred to react；When colloidal sol proportion reaches 1.700~1.750, it is added
It is equivalent to the stabilizer of raw material antimony oxide quality 2.20~2.80%, is stirred to react.
8. according to the preparation method of one of claim 1~7 low viscosity antimony pentoxide hydrosol, it is characterised in that：Step
Suddenly（2）In, the cooling immediately refers to being cooled to≤60 DEG C in 20~30min.
9. according to the preparation method of one of claim 1~8 low viscosity antimony pentoxide hydrosol, it is characterised in that：Step
Suddenly（2）In, pH value is adjusted to 6.1~6.8 with alkaline matter；The alkaline matter is triethanolamine, diethanol amine or an ethyl alcohol
One or more of amine.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603923A (en) * | 2018-12-18 | 2019-04-12 | 山东益丰生化环保股份有限公司 | A kind of preparation method of catalytic cracking double-metal deactivator |
| CN111748231A (en) * | 2020-06-28 | 2020-10-09 | 四川硅迪新材料有限公司 | Synthesis method of antimony oxide sol and flame-retardant auxiliary |
| CN113060763A (en) * | 2021-03-18 | 2021-07-02 | 刘明钢 | Preparation method of powdery antimony pentoxide applied to optical glass |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02180717A (en) * | 1988-12-28 | 1990-07-13 | Catalysts & Chem Ind Co Ltd | Antomony oxide sol and its production |
| CN1074945A (en) * | 1992-01-28 | 1993-08-04 | 锡矿山矿务局 | Chlorinolysis is produced colloidal antimony pentoxide |
| KR20030044442A (en) * | 2001-11-30 | 2003-06-09 | 홍기철 | Improved method for preparation of antimony-containing flame retardant |
| CN1456511A (en) * | 2002-05-07 | 2003-11-19 | 日产化学工业株式会社 | Antimonic oxide sol preparing method |
| CN1544338A (en) * | 2003-11-11 | 2004-11-10 | 清华大学 | Antimony peroxide ethanol dispersion preparation method |
| CN1544339A (en) * | 2003-11-11 | 2004-11-10 | 清华大学 | Antimony pentoxide dispersion preparation method |
| CN101023030A (en) * | 2004-09-21 | 2007-08-22 | 日产化学工业株式会社 | Process for producing antimony pentaoxide |
| CN101798112A (en) * | 2010-03-25 | 2010-08-11 | 中南大学 | Method for preparing antimony pentoxide hydrosol and dry powder thereof by using composite stabilizer |
| CN104030354A (en) * | 2014-06-27 | 2014-09-10 | 锡矿山闪星锑业有限责任公司 | Preparation method of hydrophobic organic antimony pentoxide sol and powder |
| CN104591279A (en) * | 2013-10-30 | 2015-05-06 | 青岛旺裕橡胶制品有限公司 | Direct method used for preparing antimony pentoxide organosol |
| CN104828866A (en) * | 2015-06-09 | 2015-08-12 | 锡矿山闪星锑业有限责任公司 | Colloidal antimony oxide powder low in volatility at high temperature and preparing method thereof |
-
2018
- 2018-09-21 CN CN201811104523.5A patent/CN108793250B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02180717A (en) * | 1988-12-28 | 1990-07-13 | Catalysts & Chem Ind Co Ltd | Antomony oxide sol and its production |
| CN1074945A (en) * | 1992-01-28 | 1993-08-04 | 锡矿山矿务局 | Chlorinolysis is produced colloidal antimony pentoxide |
| KR20030044442A (en) * | 2001-11-30 | 2003-06-09 | 홍기철 | Improved method for preparation of antimony-containing flame retardant |
| CN1456511A (en) * | 2002-05-07 | 2003-11-19 | 日产化学工业株式会社 | Antimonic oxide sol preparing method |
| CN1544338A (en) * | 2003-11-11 | 2004-11-10 | 清华大学 | Antimony peroxide ethanol dispersion preparation method |
| CN1544339A (en) * | 2003-11-11 | 2004-11-10 | 清华大学 | Antimony pentoxide dispersion preparation method |
| CN101023030A (en) * | 2004-09-21 | 2007-08-22 | 日产化学工业株式会社 | Process for producing antimony pentaoxide |
| CN101798112A (en) * | 2010-03-25 | 2010-08-11 | 中南大学 | Method for preparing antimony pentoxide hydrosol and dry powder thereof by using composite stabilizer |
| CN104591279A (en) * | 2013-10-30 | 2015-05-06 | 青岛旺裕橡胶制品有限公司 | Direct method used for preparing antimony pentoxide organosol |
| CN104030354A (en) * | 2014-06-27 | 2014-09-10 | 锡矿山闪星锑业有限责任公司 | Preparation method of hydrophobic organic antimony pentoxide sol and powder |
| CN104828866A (en) * | 2015-06-09 | 2015-08-12 | 锡矿山闪星锑业有限责任公司 | Colloidal antimony oxide powder low in volatility at high temperature and preparing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 朱洪法编著: "《精细化工产品配方与制造》", 31 October 1994, 北京：金盾出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603923A (en) * | 2018-12-18 | 2019-04-12 | 山东益丰生化环保股份有限公司 | A kind of preparation method of catalytic cracking double-metal deactivator |
| CN111748231A (en) * | 2020-06-28 | 2020-10-09 | 四川硅迪新材料有限公司 | Synthesis method of antimony oxide sol and flame-retardant auxiliary |
| CN113060763A (en) * | 2021-03-18 | 2021-07-02 | 刘明钢 | Preparation method of powdery antimony pentoxide applied to optical glass |
| CN113060763B (en) * | 2021-03-18 | 2022-11-29 | 刘明钢 | Preparation method of powdery antimony pentoxide applied to optical glass |
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