CN106957539A - A kind of production method of high near-infrared reflection ratio titanium brown - Google Patents
A kind of production method of high near-infrared reflection ratio titanium brown Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention discloses a kind of production method of high near-infrared reflection ratio titanium brown.The present invention utilizes the high reaction activity of nanoscale hydrated titanium dioxide, from suitable nanoscale hydrated titanium dioxide, the additive such as addition titanic acid-sol, Zn-ef ficiency, antimony oxide, phosphoric acid, chromium oxide, by high-temperature calcination, crush, high near-infrared reflection ratio titanium brown product is made in desalination.The product has the notable feature that rational particle diameter distribution, color are moderate, easy scattered, near-infrared reflection ratio is high, is the ideal product of brown color near-infrared reflection functional material.
Description
Technical field
The present invention relates to the preparation method of titanium brown, Gao Jinhong is prepared more particularly, to using suitable nanoscale hydrated titanium dioxide
Production method of the external reflectance than titanium brown.
Background technology
Power-saving technology is paid attention to increasingly both at home and abroad at present, it is a kind of easy to be easy to improve to the direct albedo of solar radiation
Capable technology path.From the point of view of the Energy distribution of the sun, the wavelength for the solar radiant energy that can be received on the earth is mainly distributed
In the range of 250~2500nm, three parts can be divided into, the wave-length coverage of each part and shared energy are respectively:It is small
The 3% of gross energy is accounted in 380nm ultraviolet region;380~780nm visible region accounts for the 45% of gross energy;It is more than
780nm near infrared region accounts for the 52% of gross energy.The wavelength for producing the main solar radiant energy of fuel factor is more than 780nm's
Near infrared region, improves the direct reflection near infrared region solar radiant energy, can play the effect of cooling consumption reduction.
Traditional color pigment, it is impossible to adapt to the high near-infrared reflection ability of power conservation requirement, it is impossible to meet energy-saving function
Products application requirement.Titanium brown with rutile crystal form can then have high near when rational particle diameter distribution is arrived in control
Infrared external reflection ratio, is one of comparatively ideal colored near-infrared reflection functional material.
The excellent properties that titanium brown has:1. due to being got by pyroreaction and calcining, with rutile-type crystal formation, lattice
Stability Analysis of Structures, heat-resisting, fast light, weather-proof and resistance to various chemical mediator performances are very excellent, and anti-grinded hardness index is good.2. titanium brown has
Neutral pH value, it is adaptable to various medium systems, will not react with medium system.3. the color development element that titanium brown contains enters
TiO2The security system of nontoxicization requirement is not completely suitable for by any medium etch under lattice, general condition.
The more ripe titanium brown product of in the market more use solid phase method technique, using titanium dioxide as primary raw material, although technique compared with
To be simple, cost is relatively low, but because titanium dioxide has been stable crystal structure, it is necessary to which higher temperature carries out soild oxide
Mixed calcining, causes unstable product quality.It is that primary raw material carries out titanium brown using nanoscale high activity hydrated titanium dioxide
The other mixing of molecular level is realized between production, material, is a kind of simple and easy to do and stably and controllable product quality production method.
The content of the invention
The purpose of the present invention, is to provide for a kind of production method of high near-infrared reflection ratio titanium brown, what this method was solved
The characteristics of technical problem is the high reaction activity using nanoscale hydrated titanium dioxide, realizes between material it is that molecular level is other mixed
Close.Once washing, acid treatment, secondary water are carried out by preferred nanoscale high activity hydrated titanium dioxide, to hydrated titanium dioxide
Wash, add inorganic agent mixing, calcining, once crush, grind the key steps such as desalination, drying, steam flow crushing, to reach that output is high near
Purpose of the infrared external reflection than titanium brown.
The production method that the present invention is provided comprises the steps:
A, hydrated titanium dioxide are once washed:Choose hydrolysate hydration titanium dioxide prepared by sulfate process titanium dioxide production technology
Titanium, sedimentation rate index meets 150~200mm/20min, and hydrated titanium dioxide is washed with 55~70 DEG C of running water, washing
Qualified Judging index is that the iron content (in terms of Fe) in a washing waste water is less than 100mg/L;
B, acid treatment:Gained hydrated titanium dioxide will once be washed plus slurry, titanium dioxide concentration control is made in running water
For 320~380g/L, temperature is at 55~70 DEG C, with H2SO4Meter, addition sulfuric acid is 30~50g/L, with Ti2O3Count, titanous is
0.5~1.5g/L, handles slurry 1~2 hour on this condition;After processing terminates, TiO in calcining seeds, calcining seeds is added2
Quality account in pending slurry contained TiO2The 2~7% of quality, are stirred 30 minutes;
The calcining seeds are titanic acid-sol calcining seeds, and the titanic acid-sol calcining seeds are given birth to for sulfate process titanium dioxide
Rutile type calcining seeds prepared by production. art;
The secondary washing of c, hydrated titanium dioxide:With 55~70 DEG C of desalted waters hydrated titanium dioxide good to step b acid treatments
Slurry is washed, and the qualified Judging index of washing is the iron content in secondary washing waste water (with Fe2O3Meter) control less than
10mg/L。
D plus inorganic agent:Desalted water is added to adjust titanium dioxide concentration control in hydrated titanium dioxide slurry obtained by secondary washing
For 320~380g/L;Slurry pH value is adjusted to 2.5~4.0 with alkali;To account for contained TiO in pending slurry2The mass fraction of amount
Meter, with Sb2O3Meter, the adding proportion of antimony oxide is 10~15%;With Cr2O3Meter, the adding proportion of chromium oxide is 5~10%;With
H3PO4Meter, the adding proportion of phosphoric acid is 0.00~0.25%;In terms of ZnO, the adding proportion of zinc oxide or zinc sulfate or zinc chloride
For 0.0~0.5%;In terms of MgO, the adding proportion of magnesia or magnesium sulfate or magnesium chloride is 0.0~0.5%;Add above-mentioned examination
Slurry is stirred after agent 0.5~1 hour, slurry is pressed dry into moisture standby.
E, calcining:The material for pressing dry moisture is calcined, highest calcining heat is controlled between 900~1200 DEG C, is forged
Rutile-type crystal formation content >=98.5% in burning product;
F, crushing:Calcining product are crushed with pulverizer, 45 μm of residue on sieves of control smashing fineness are less than 0.05%, produce
High near-infrared reflection ratio titanium brown primary product;
G, desalination, sand milling:Slurry is made with desalted water in titanium brown primary product, slurry is ground with sand mill, is selected
With 1.2~1.4 μm of zirconium silicate pearls or yttrium stabilised zirconia pearl, the slurry after grinding is washed with desalted water, control washing is useless
Water conductivity is less than 80 μm/cm, slurry is pressed dry into moisture standby;
H, drying, steam flow are crushed:The drying materials for pressing dry moisture are removed into moisture removal, trimethylolethane, three hydroxyl first are added
Base propane, polydimethylsiloxanepolymer polymer one kind therein, addition is account for comminuting matter quality 0.1~0.8%, through vapour
Stream crushes to obtain titanium brown product.
Beneficial effects of the present invention are:
(1) products obtained therefrom of the present invention is rutile-type crystal structure, and with preferable particle diameter distribution, particle diameter D50 is between 500
Between~1500nm, product has excellent near infrared ray reflective ability.This method is hydrated dioxy by preferred nanoscale high activity
Change titanium and color development element, auxiliary agent simultaneously added after carrying out removal of impurities to it, realize between material it is the other mixing of molecular level so that
The size tunable growth of titanium brown product;, can by carrying out desalination to primary product, grinding and adding different surfactants
So that product has wider applicability.
(2) present invention process is simple, easy to operate, with low cost.
Embodiment
With reference to specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to
This.
Embodiment 1
The hydrolysate hydrated titanium dioxide for taking sulfate process titanium dioxide production technology to prepare, sedimentation rate is 155mm/20min, with
55~60 DEG C of running water are washed to hydrated titanium dioxide, iron content (in terms of Fe) 95mg/L in a washing waste water;Will
Once washing gained hydrated titanium dioxide adds running water that slurry is made, and concentration is 322g/L, and temperature adds sulfuric acid at 60~65 DEG C
(with H2SO4Meter) it is 48g/L, titanous is (with Ti2O3Meter) it is 0.6g/L, it is contained in pending slurry to account for after handling 1 hour
TiO2The mass fraction meter of amount, adds titanic acid-sol calcining seeds (with TiO2Meter), adding proportion is 2%;It is de- with 60~65 DEG C
The salt solution hydrated titanium dioxide good to acid treatment is washed, and the iron content in secondary washing waste water is (with Fe2O3Meter) it is 8mg/L;
Add desalted water that slurry is made hydrated titanium dioxide obtained by secondary washing, concentration is 335g/L;With potassium hydroxide adjustment slurry PH
It is worth 2.5~4.0;To account for contained TiO in pending slurry2The mass fraction meter of amount, the antimony oxide of addition is (with Sb2O3Meter) add
Plus ratio is 10%;Chromium oxide is (with Cr2O3Meter) adding proportion be 5%;Phosphoric acid is (with H3PO4Meter) adding proportion be 0.25%;Oxygen
Change zinc or zinc sulfate or zinc chloride (counts) adding proportion as 0.5% using ZnO;Add and stirred 0.5~1 hour after mentioned reagent, will
Slurry press dry moisture and calcined, and highest calcining heat control rutile-type crystal formation content in 1150 DEG C, calcining product is
99.5%;Calcining product are crushed with mechanical crusher, smashing fineness 0.02%, produce high near-infrared reflection ratio titanium brown primary
Product;Slurry is made with desalted water in titanium brown primary product, slurry is ground with sand mill, from 1.2~1.4 μm of silicon
Sour zirconium pearl, is washed with desalted water to the slurry after grinding, 75 μm/cm of washing waste water electrical conductivity, and slurry is pressed dry into moisture;Will
The drying materials for pressing dry moisture remove moisture removal, add trimethylolethane, addition is account for comminuting matter quality 0.1%, warp
Steam flow crushes to obtain high near-infrared reflection ratio titanium brown product.
Embodiment 2
The hydrolysate hydrated titanium dioxide for taking sulfate process titanium dioxide production technology to prepare, sedimentation rate is 195mm/20min, with
60~65 DEG C of running water are washed to hydrated titanium dioxide, iron content (in terms of Fe) 85mg/L in a washing waste water;Will
Once washing gained hydrated titanium dioxide adds running water that slurry is made, and concentration is 375g/L, and temperature adds sulfuric acid at 55~60 DEG C
(with H2SO4Meter) it is 32g/L, titanous is (with Ti2O3Meter) it is 1.5g/L, it is contained in pending slurry to account for after handling 2 hours
TiO2The mass fraction meter of amount, adds titanic acid-sol calcining seeds (in terms of TiO2), adding proportion is 7%;With 60~65 DEG C
The desalted water hydrated titanium dioxide good to acid treatment is washed, and the iron content in secondary washing waste water is (with Fe2O3Meter) be
10mg/L;Add desalted water that slurry is made hydrated titanium dioxide obtained by secondary washing, concentration is 360g/L;Adjusted and starched with potassium carbonate
Expect pH value to 2.5~4.0;To account for contained TiO in pending slurry2The mass fraction meter of amount, the antimony oxide of addition is (with Sb2O3
Meter) adding proportion be 15%;Chromium oxide is (with Cr2O3Meter) adding proportion be 10%;Phosphoric acid is (with H3PO4Meter) adding proportion is
0.00%;Zinc oxide or zinc sulfate or zinc chloride (count) adding proportion as 0.0% using ZnO;Magnesia or magnesium sulfate or magnesium chloride
Adding proportion is 0.5%;Add and stirred 0.5~1 hour after mentioned reagent, slurry is pressed dry into moisture and calcined, highest calcining
Temperature control rutile-type crystal formation content in 900 DEG C, calcining product is 98.5%;Calcining product are subjected to powder with mechanical crusher
Broken, smashing fineness 0.04% produces high near-infrared reflection ratio titanium brown primary product;Slurry is made of desalted water for titanium brown primary product
Material, is ground to slurry with sand mill, from 1.2~1.4 μm of yttrium stabilised zirconia pearl, the slurry after grinding is entered with desalted water
Water-filling is washed, 75 μm/cm of washing waste water electrical conductivity, and slurry is pressed dry into moisture;The drying materials for pressing dry moisture are removed into moisture removal, added
Trimethylolpropane, addition is account for comminuting matter quality 0.3%, and high near-infrared reflection ratio titanium brown production is crushed to obtain through steam flow
Product.
Embodiment 3
The hydrolysate hydrated titanium dioxide for taking sulfate process titanium dioxide production technology to prepare, sedimentation rate is 170mm/20min, with
55~60 DEG C of running water are washed to hydrated titanium dioxide, iron content (in terms of Fe) 85mg/L in a washing waste water;Will
Once washing gained hydrated titanium dioxide adds running water that slurry is made, and concentration is 352g/L, and temperature adds sulfuric acid at 65~70 DEG C
(with H2SO4Meter) it is 35g/L, titanous is (with Ti2O3Meter) it is 1.1g/L, it is contained in pending slurry to account for after handling 1.5 hours
The mass fraction meter of TiO2 amounts, adds titanic acid-sol calcining seeds (with TiO2Meter), adding proportion is 5%;With 55~60 DEG C
The desalted water hydrated titanium dioxide good to acid treatment is washed, and the iron content in secondary washing waste water is (with Fe2O3Meter) it is 9mg/
L;Add desalted water that slurry is made hydrated titanium dioxide obtained by secondary washing, concentration control is 360g/L;Adjusted with NaOH
Slurry pH value is to 2.5~4.0;To account for contained TiO in pending slurry2The mass fraction meter of amount, the antimony oxide of addition is (with Sb2O3
Meter) adding proportion be 12%;Chromium oxide is (with Cr2O3Meter) adding proportion be 8%;Phosphoric acid is (with H3PO4Meter) adding proportion is
0.05%;Zinc oxide or zinc sulfate or zinc chloride (count) adding proportion as 0.3% using ZnO;Magnesia or magnesium sulfate or magnesium chloride
Adding proportion is 0.2%;Add and stirred 0.5~1 hour after mentioned reagent, slurry is pressed dry into moisture and calcined, highest calcining
Temperature control rutile-type crystal formation content >=99.0% in 1000 DEG C, calcining product;Calcining product are subjected to powder with mechanical crusher
Broken, smashing fineness 0.04% produces high near-infrared reflection ratio titanium brown primary product;Slurry is made of desalted water for titanium brown primary product
Material, is ground to slurry with sand mill, from 1.2~1.4 μm of zirconium silicate pearl, the slurry after grinding is carried out with desalted water
Slurry is pressed dry moisture by washing, 78 μm/cm of washing waste water electrical conductivity;The drying materials for pressing dry moisture are removed into moisture removal, added poly-
Dimethylsiloxane polymer, addition is account for comminuting matter quality 0.8%, and high near-infrared reflection ratio titanium is crushed to obtain through steam flow
Brown product.
The titanium brown product of embodiment is detected, R% therein is XRD testing results, particle diameter is examined for laser particle analyzer
Result is surveyed, near-infrared reflection ratio (NIR) is the testing results of Agilent cary 5000, and gained detection data are arranged in table 1 later
Show:
Table 1:Embodiment Product checking data
Claims (10)
1. a kind of production method of high near-infrared reflection ratio titanium brown, it is characterised in that comprise the following steps:
A, hydrated titanium dioxide are once washed:Take qualified hydrolysate hydration titanium dioxide prepared by sulfate process titanium dioxide production technology
Titanium, is washed with 50~60 DEG C of running water to hydrated titanium dioxide, washes qualified Judging index in a washing waste water
Iron content (in terms of Fe) be less than 100mg/L;
B, acid treatment:Gained hydrated titanium dioxide will once be washed plus slurry is made in running water, titanium dioxide concentration control is 320
~380g/L, temperature is at 55~70 DEG C, with H2SO4Meter, addition sulfuric acid is 30~50g/L;With Ti2O3Meter, titanous be 0.5~
1.5g/L, handles slurry 1~2 hour on this condition;After processing terminates, TiO in calcining seeds, calcining seeds is added2Matter
Measure to account for contained TiO in pending slurry2The 2~7% of quality, are stirred 30 minutes after adding;
The secondary washing of c, hydrated titanium dioxide:With 55~70 DEG C of desalted waters hydrated titanium dioxide slurry good to step b acid treatments
Washed, the qualified Judging index of washing is the iron content in secondary washing waste water (with Fe2O3Meter) control less than 10mg/
L;
D plus inorganic agent:Add desalted water to adjust titanium dioxide concentration control in hydrated titanium dioxide slurry obtained by secondary washing to be
320~380g/L;Slurry pH value is adjusted to 2.5~4.0 with alkali;To account for contained TiO in pending slurry2The mass fraction of amount
Meter, with Sb2O3Meter, the adding proportion of antimony oxide is 10~15%;With Cr2O3Meter, the adding proportion of chromium oxide is 5~10%;With
H3PO4Meter, the adding proportion of phosphoric acid is 0.00~0.25%;In terms of ZnO, the adding proportion in zinc source is 0.0~0.5%;With MgO
Meter, the adding proportion in magnesium source is 0.0~0.5%;Add and stirred 0.5~1 hour after mentioned reagent, slurry is pressed dry into moisture standby
With;
E, calcining:The material for pressing dry moisture is calcined, highest calcining heat is controlled between 900~1200 DEG C, and control is forged
Rutile-type crystal formation content >=98.5% in burning product;
F, crushing:Calcining product are crushed with pulverizer, control smashing fineness is qualified, at the beginning of producing high near-infrared reflection ratio titanium brown
Level product;
G, desalination, sand milling:Slurry is made with desalted water in titanium brown primary product, slurry is ground with sand mill, from 1.2
~1.4 μm of zirconium silicate pearl or yttrium stabilised zirconia pearl, is washed with desalted water to the slurry after grinding, controls washing waste water conductance
Rate is less than 80 μm/cm, slurry is pressed dry into moisture standby;
H, drying, steam flow are crushed:The drying materials for pressing dry moisture are removed into moisture removal, surface conditioning agent is added, is crushed through steam flow
High near-infrared reflection ratio titanium brown product.
2. a kind of production method of high near-infrared reflection ratio titanium brown according to claims 1, it is characterised in that step a
In, qualified hydrolysate hydrated titanium dioxide prepared by the sulfate process titanium dioxide production technology refers to hydrolysate sedimentation rate index
Meet 150~200mm/20min hydrolysis material;The measuring method of hydrolysate sedimentation rate index is:100ml is taken to be more than 90 DEG C
Hydrolysate and 900ml temperature be sufficiently mixed for 20 ± 2 DEG C of desalted water after, be placed in 1000ml graduated cylinders, in 22 ± 2 DEG C
Standing sedimentation 20min under environment, the supernatant liquor measured highly is the hydrolysate sedimentation rate.
3. a kind of production method of high near-infrared reflection ratio titanium brown according to claims 1, it is characterised in that step b
In, the calcining seeds are titanic acid-sol calcining seeds, and the titanic acid-sol calcining seeds are that sulfate process titanium dioxide produces work
Rutile type calcining seeds prepared by skill.
4. a kind of production method of high near-infrared reflection ratio titanium brown according to claims 1 or 2, it is characterised in that institute
State desalted water and meet electrical conductivity less than 10 μ s/cm, clear appearance is transparent.
5. the production method of a kind of high near-infrared reflection ratio titanium brown according to claim 1, it is characterised in that in step d,
The alkali is potassium hydroxide, potassium carbonate, NaOH, sodium carbonate one kind therein;The antimony oxide refers to content (with Sb2O3Meter)
>=99.0%, the industrial goods antimony oxide of residue on sieve (mass fraction, 45 μm)≤0.05%;The chromic oxide content is (with Cr2O3Meter)
>=99%, the industrial goods chromium oxide of residue on sieve (mass fraction, 45 μm)≤0.01%.
6. the production method of a kind of high near-infrared reflection ratio titanium brown according to claim 1, it is characterised in that in step d,
The zinc source is zinc oxide, zinc sulfate or zinc chloride;Magnesium source is magnesia, magnesium sulfate or magnesium chloride.
7. the production method of a kind of high near-infrared reflection ratio titanium brown according to claim 1, it is characterised in that in step f,
The smashing fineness is qualified, produces high near-infrared reflection ratio titanium brown primary product and refers to that 45 μm of residue on sieves are less than 0.05%, through swashing
Light particle size analyzer detects particle diameter D50 between 500~1500nm, the pulverized product of rutile-type crystal formation content >=98.5%.
8. the production method of a kind of high near-infrared reflection ratio titanium brown according to claim 1, it is characterised in that in step h,
The surface conditioning agent is trimethylolethane, trimethylolpropane, polydimethylsiloxanepolymer polymer one kind therein, addition
Measure to account for 0.1~0.8% (mass ratio) of comminuting matter quality.
9. the production method of a kind of high near-infrared reflection ratio titanium brown according to claim 1, it is characterised in that in step h,
The high near-infrared reflection ratio titanium brown product refers to that 45 μm of residue on sieves are less than 0.02%, detects that particle diameter D50 is situated between through laser particle analyzer
Between 500~1500nm, water dissolvable salt content is less than 0.1%, the pulverized product of rutile-type crystal formation content >=98.5%.
10. the purposes of high near-infrared reflection ratio titanium brown according to made from preparation method according to any one of claims 1 to 9,
Characterized in that, the high near-infrared reflection ratio titanium brown product to be used for the pale brown color system for needing to reflect near infrared ray.
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CN108165052A (en) * | 2017-12-14 | 2018-06-15 | 华南理工大学 | A kind of ceramic pigment with near-infrared reflection and preparation method thereof |
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