CN109867987A - A kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material - Google Patents
A kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material Download PDFInfo
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- CN109867987A CN109867987A CN201910209103.1A CN201910209103A CN109867987A CN 109867987 A CN109867987 A CN 109867987A CN 201910209103 A CN201910209103 A CN 201910209103A CN 109867987 A CN109867987 A CN 109867987A
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Abstract
A kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material, belongs to field of inorganic materials.The present invention is cleaned first by collision friction pretreatment to cenosphere and roughing in surface, then pass through surfactant modified and heterogeneous hydrothermal reaction at low temperature, one step grows the high infrared reflection red schorl phase titanium dioxide clad of even compact on cenosphere surface, to substitute existing anatase titanium dioxide clad, realize that the infrared reflectivity of cenosphere further increases, it is final that the infrared reflective material with high reflection heat-proof quality is made.Cenosphere surface prepared by the present invention surrounding phase is red schorl phase titanium dioxide, has more excellent properties of infrared reflection compared to anatase phase titanium dioxide.One-step synthesis red schorl phase titanium dioxide coats microballon, is not required to carry out crystal transfer by high-temperature calcination, can substantially energy saving.
Description
Technical field
The present invention relates to a kind of red schorl phase titanium dioxide cladding cenosphere infrared external reflection heat-barrier material preparation method,
Belong to field of inorganic materials.
Technical background
Cenosphere is a kind of thin-wall ball with special hollow structure, since its surface is smooth, symmetrical configuration, inside
Vacuum or filled with N2、CO2Equal gases, therefore there is excellent dispersed, good mobility, extremely low density and lower heat
The advantages that conductance, is widely used in the fields such as building, aviation in recent years.Cenosphere is mixed with resin can be made into thermal insulation
Energy is good, small in size, density is low, the heat insulating coatings with certain flame retardant property, can solve existing traditional organic foam
Poor, the inflammable disadvantage of heat-barrier material weatherability.Although cenosphere can largely reduce thermal conduction rate, it inclines
To in absorbing and transmitting the infrared light in sunlight, this causes its temperature that can obviously rise as sunlight irradiates, and substantially influences
Its heat insulation.
For the above status, there is work to attempt to solve relevant issues.Chinese patent ZL200610127227.8 is disclosed
Filler and insulating moulding coating of a kind of coated by titanium dioxide fly ash float and preparation method thereof, the material is by using having height
The titanium dioxide of infrared reflection performance coats fly ash micro-sphere, and the infrared reflective of cenosphere is greatly improved
Can, but titanium dioxide includes a variety of crystal forms, the red schorl phase titanium dioxide for not using properties of infrared reflection most excellent
It is coated, there are also rooms for promotion for properties of infrared reflection.Chinese patent ZL201410309881.5 disclose a kind of titanium dioxide/
Cenosphere composite particles, sunlight reflective insulation filler, coating and preparation method thereof, the material will be at by sol-gal process
Product red schorl phase titanium dioxide particle and cenosphere bond, but also wrap during the bonding process on red schorl phase titanium dioxide surface
Layer of silicon dioxide has been covered, the infrared reflectivity of red schorl phase titanium dioxide is affected.
Summary of the invention
In view of the foregoing drawbacks, the present invention provides a kind of red schorl phase titanium dioxide cladding heat-insulated material of cenosphere infrared external reflection
Material is pre-processed by collision friction carry out cleaning and roughing in surface to cenosphere first, then by surfactant modified
And heterogeneous hydrothermal reaction at low temperature, a step grow the high infrared reflection Rutile Type dioxy of even compact on cenosphere surface
Change titanium clad, to substitute existing anatase titanium dioxide clad, realizes the infrared reflectivity of cenosphere into one
Step improves, final that the infrared reflective material with high reflection heat-proof quality is made.
A kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material, it is characterised in that including following step
It is rapid:
(1) cleaning and roughing in surface: certain mass cenosphere is placed in tank body, tank body is with 500~5000 revs/min
High speed rotation, cenosphere, by mutual collision friction, remove bead surface attachment and increase its surface in tank interior
Roughness, tank body stop after rotating 0.5~6 hour, take out boring microballon, and obtained cleaning is hollow micro- with roughing in surface
Pearl；
(2) surface modification: cleaning and the cenosphere, surfactant, water of roughing in surface are carried out by certain mass ratio
Ingredient is weighed, mixture liquid temperature is adjusted after mixing and is reacted to 1~50 DEG C, the reaction time is 5~60 minutes, is reacted
It is 100~1500 revs/min that speed of agitator is controlled in journey, and cenosphere is taken out in filtering after reaction, is placed at 120 DEG C dry
The modified cenosphere in surface is made after drying in 2 hours；
(3) synthesis cladding: carrying out weighing ingredient by certain mass ratio for the modified cenosphere in surface, titanium source, hydrochloric acid, water,
It is 1~10 DEG C that mixture liquid temperature is controlled in mixed process, and 30~95 DEG C are heated to after mixing and is reacted, the reaction time is
0.5~12 hour, it was 100~1500 revs/min that speed of agitator is controlled in reaction process, and filtering is taken out hollow micro- after reaction
Pearl is placed at 80 DEG C dry 2 hours and is dried, then calcined using distilled water flushing to neutrality, and rutile is made after cooling
Phase titanic oxide coats cenosphere infrared external reflection heat-barrier material.
Further, the cenosphere added in tank body described in step 1, volume account for the 3~40% of tank volume.
Further, cenosphere diameter range described in step 1 is 5~400 microns.
Further, 3 kinds of components of cenosphere, surfactant, water of cleaning and roughing in surface described in step 2 according to
Following parts by weight mixing:
The cenosphere 250~1500 of cleaning and roughing in surface；
Surfactant 1~7；
Water 1000~50000.
Further, surfactant described in step 2 is glycidol triethylammonium chloride, N- lauroyl flesh ammonia
The combination of one or more of sour sodium, cetyl trimethylammonium bromide.
Further, 4 kinds of modified cenosphere in surface described in step 3, titanium source, hydrochloric acid, water components are according to following weight
Number mixing:
Further, titanium source described in step 3 is the combination of one or more of titanium tetrachloride, titanium sulfate, titanyl sulfate.
Further, calcinating system described in step 3 are as follows: be warming up to 200~400 DEG C with 3 DEG C/min and heat preservation 2~6 is small
When.
The invention has the advantages that (1) cenosphere surface surrounding phase is red schorl phase titanium dioxide, compared to Anatase
Titanium dioxide has more excellent properties of infrared reflection.(2) one-step synthesis red schorl phase titanium dioxide coats microballon, is not required to through excessively high
Temperature calcining carries out crystal transfer, can substantially energy saving.
Detailed description of the invention:
Fig. 1 is a kind of red schorl phase titanium dioxide cladding cenosphere infrared external reflection heat-barrier material prepared by embodiment 1
Stereoscan photograph, cenosphere surface coating layer even compact, no breakage fall off as seen from the figure.
Specific embodiment
Clear and complete description is done to the present invention with reference to the accompanying drawing, so that those skilled in the art is not needing to make
Under conditions of creative work, it can sufficiently implement the present invention.
A specific embodiment of the invention is as follows:
Embodiment 1:(1) in tank body add total volume be tank volume 15% cenosphere (250 microns), tank body with
3700 revs/min of high speed rotations, cenosphere in tank interior by mutual collision friction, remove bead surface attachment and
Increase its surface roughness, tank body stops after rotating 0.5 hour, takes out boring microballon, and cleaning and roughing in surface is made
Cenosphere；(2) cenosphere, the 4 parts of N- lauroyl sarcosines of 500 parts of cleanings and roughing in surface are weighed according to parts by weight
Sodium, 1000 parts of water carry out weighing ingredient by certain mass ratio, and mixture liquid temperature is adjusted after mixing and is reacted to 1 DEG C, instead
It is 15 minutes between seasonable, it is 1250 revs/min that speed of agitator is controlled in reaction process, and filtering is taken out hollow micro- after reaction
The modified cenosphere in surface is made after being placed at 120 DEG C drying in dry 2 hours in pearl；(3) 12 parts of surfaces are weighed according to parts by weight
Modified cenosphere, 3 parts of titanium tetrachlorides, 35 parts of hydrochloric acid, 2500 parts of water carry out weighing ingredient by certain mass ratio, in mixed process
Controlling mixture liquid temperature is 8 DEG C, and 47 DEG C are heated to after mixing and is reacted, and the reaction time is 0.5 hour, in reaction process
Controlling speed of agitator is 1500 revs/min, and filtering is taken out cenosphere and set using distilled water flushing to neutrality after reaction
It dries within dry 2 hours at 80 DEG C, is then warming up to 275 DEG C with 3 DEG C/min and keeps the temperature 3.5 hours and calcined, made after cooling
It obtains red schorl phase titanium dioxide and coats cenosphere.
Embodiment 2:(1) in tank body add total volume be tank volume 3% cenosphere (350 microns), tank body with
2500 revs/min of high speed rotations, cenosphere in tank interior by mutual collision friction, remove bead surface attachment and
Increase its surface roughness, tank body stops after rotating 1.5 hours, takes out boring microballon, and cleaning and roughing in surface is made
Cenosphere；(2) cenosphere, 5 parts of three second of glycidyl of 1250 parts of cleanings and roughing in surface are weighed according to parts by weight
Ammonium chloride, 3000 parts of water carry out weighing ingredient by certain mass ratio, and mixture liquid temperature is adjusted after mixing to 40 DEG C of progress
Reaction, reaction time are 60 minutes, and it is 700 revs/min that speed of agitator is controlled in reaction process, and filtering is taken out empty after reaction
The modified cenosphere in surface is made after being placed at 120 DEG C drying in dry 2 hours in heart microballon；(3) 5 parts are weighed according to parts by weight
Surface is modified cenosphere, 41 parts of titanium sulfates, 8 parts of hydrochloric acid, 1450 parts of water and carries out weighing ingredient, mixed process by certain mass ratio
Middle control mixture liquid temperature is 3 DEG C, and 95 DEG C are heated to after mixing and is reacted, and the reaction time is 10.5 hours, is reacted
It is 600 revs/min that speed of agitator is controlled in journey, and cenosphere is taken out in filtering after reaction, using distilled water flushing to neutrality,
It is placed at 80 DEG C dry 2 hours and dries, be then warming up to 200 DEG C with 3 DEG C/min and keep the temperature 6 hours and calcined, made after cooling
It obtains red schorl phase titanium dioxide and coats cenosphere.
Embodiment 3:(1) in tank body add total volume be tank volume 40% cenosphere (75 microns), tank body with
1350 revs/min of high speed rotations, cenosphere in tank interior by mutual collision friction, remove bead surface attachment and
Increase its surface roughness, tank body stops after rotating 6 hours, takes out boring microballon, and the sky of cleaning with roughing in surface is made
Heart microballon；(2) cenosphere, the 1 part of cetyl trimethyl bromine of 1500 parts of cleanings and roughing in surface are weighed according to parts by weight
Change ammonium, 50000 parts of water by certain mass ratio carry out weighing ingredient, mixture liquid temperature is adjusted after mixing and is reacted to 8 DEG C,
Reaction time is 30 minutes, and it is 100 revs/min that speed of agitator is controlled in reaction process, and filtering is taken out hollow micro- after reaction
The modified cenosphere in surface is made after being placed at 120 DEG C drying in dry 2 hours in pearl；(3) 3 parts of surfaces are weighed according to parts by weight
Modified cenosphere, 6 parts of titanyl sulfates, 14 parts of hydrochloric acid, 3000 parts of water carry out weighing ingredient by certain mass ratio, in mixed process
Controlling mixture liquid temperature is 6 DEG C, and 85 DEG C are heated to after mixing and is reacted, and the reaction time is 12 hours, in reaction process
Controlling speed of agitator is 100 revs/min, and filtering is taken out cenosphere and is placed in using distilled water flushing to neutrality after reaction
It dries within dry 2 hours at 80 DEG C, is then warming up to 270 DEG C with 3 DEG C/min and keeps the temperature 2 hours and calcined, gold is made after cooling
Red stone phase titanic oxide coats cenosphere.
Embodiment 4:(1) in tank body add total volume be tank volume 33% cenosphere (5 microns), tank body with
500 revs/min of high speed rotations, cenosphere in tank interior by mutual collision friction, remove bead surface attachment and
Increase its surface roughness, tank body stops after rotating 3.5 hours, takes out boring microballon, and cleaning and roughing in surface is made
Cenosphere；(2) cenosphere, the 7 parts of cetyl trimethyl bromines of 800 parts of cleanings and roughing in surface are weighed according to parts by weight
Change ammonium, 45000 parts of water and carry out weighing ingredient by certain mass ratio, it is anti-to 50 DEG C of progress that mixture liquid temperature is adjusted after mixing
It answers, the reaction time is 5 minutes, and it is 350 revs/min that speed of agitator is controlled in reaction process, and filtering is taken out hollow after reaction
The modified cenosphere in surface is made after being placed at 120 DEG C drying in dry 2 hours in microballon；(3) 19 parts of tables are weighed according to parts by weight
Face is modified cenosphere, 23 parts of titanium sulfates, 31 parts of hydrochloric acid, 200 parts of water and carries out weighing ingredient by certain mass ratio, in mixed process
Controlling mixture liquid temperature is 10 DEG C, and 39 DEG C are heated to after mixing and is reacted, and the reaction time is 4 hours, in reaction process
Controlling speed of agitator is 350 revs/min, and filtering is taken out cenosphere and is placed in using distilled water flushing to neutrality after reaction
It dries within dry 2 hours at 80 DEG C, is then warming up to 250 DEG C with 3 DEG C/min and keeps the temperature 4 hours and calcined, gold is made after cooling
Red stone phase titanic oxide coats cenosphere.
Embodiment 5:(1) in tank body add total volume be tank volume 21% cenosphere (400 microns), tank body with
5000 revs/min of high speed rotations, cenosphere in tank interior by mutual collision friction, remove bead surface attachment and
Increase its surface roughness, tank body stops after rotating 5 hours, takes out boring microballon, and the sky of cleaning with roughing in surface is made
Heart microballon；(2) cenosphere, the 2 parts of glycidyl triethyl group chlorine of 250 parts of cleanings and roughing in surface are weighed according to parts by weight
Change ammonium, 30000 parts of water and carry out weighing ingredient by certain mass ratio, it is anti-to 35 DEG C of progress that mixture liquid temperature is adjusted after mixing
It answers, the reaction time is 45 minutes, and it is 1500 revs/min that speed of agitator is controlled in reaction process, and filtering is taken out empty after reaction
The modified cenosphere in surface is made after being placed at 120 DEG C drying in dry 2 hours in heart microballon；(3) 17 parts are weighed according to parts by weight
Surface is modified cenosphere, 47 parts of titanyl sulfates, 20 parts of hydrochloric acid, 500 parts of water and carries out weighing ingredient by certain mass ratio, mixes
It is 1 DEG C that mixture liquid temperature is controlled in journey, and 30 DEG C are heated to after mixing and is reacted, and the reaction time is 6 hours, reaction process
Middle control speed of agitator is 1300 revs/min, and cenosphere is taken out in filtering after reaction, using distilled water flushing to neutrality,
It is placed at 80 DEG C dry 2 hours and dries, be then warming up to 400 DEG C with 3 DEG C/min and keep the temperature 4.5 hours and calcined, after cooling
Red schorl phase titanium dioxide is made and coats cenosphere.
Presently preferred embodiments of the present invention is described above, it should be pointed out that the invention is not limited to above-mentioned
Particular implementation, devices and structures not described in detail herein should be understood as gives reality with the common mode in this field
It applies；Anyone skilled in the art, without departing from the scope of the technical proposal of the invention, technology according to the present invention
Essence any simple modifications, equivalents, and modifications made to the above embodiment still fall within technical solution of the present invention protection
In the range of.
Claims (8)
1. a kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material, it is characterised in that including following step
It is rapid:
(1) cleaning and roughing in surface: certain mass cenosphere is placed in tank body, tank body is with 500~5000 revs/min of high speeds
Rotation, cenosphere, by mutual collision friction, remove bead surface attachment and increase its rough surface in tank interior
Degree, tank body stop after rotating 0.5~6 hour, take out boring microballon, and the cenosphere of cleaning with roughing in surface is made；
(2) surface modification: cleaning and the cenosphere, surfactant, water of roughing in surface are weighed by certain mass ratio
Ingredient adjusts mixture liquid temperature and is reacted to 1~50 DEG C after mixing, the reaction time is 5~60 minutes, in reaction process
Controlling speed of agitator is 100~1500 revs/min, and cenosphere is taken out in filtering after reaction, and it is small to be placed at 120 DEG C dry 2
When drying after the modified cenosphere in surface is made；
(3) synthesis cladding: the modified cenosphere in surface, titanium source, hydrochloric acid, water are subjected to weighing ingredient by certain mass ratio, mixed
Control mixture liquid temperature is 1~10 DEG C in the process, and 30~95 DEG C are heated to after mixing and is reacted, the reaction time 0.5
~12 hours, it was 100~1500 revs/min that speed of agitator is controlled in reaction process, and cenosphere is taken out in filtering after reaction,
It using distilled water flushing to neutrality, is placed at 80 DEG C dry 2 hours and dries, then calcined, Rutile Type is made after cooling
Coated by titanium dioxide cenosphere infrared external reflection heat-barrier material.
2. a kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material according to claim 1,
It is characterized in that the cenosphere added in tank body described in step 1, volume accounts for the 3~40% of tank volume.
3. a kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material according to claim 1,
It is characterized in that cenosphere diameter range described in step 1 is 5~400 microns.
4. a kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material according to claim 1,
It is characterized in that 3 kinds of components of cenosphere, surfactant, water of cleaning described in step 2 and roughing in surface according to following weight
Number mixing:
The cenosphere 250~1500 of cleaning and roughing in surface；
Surfactant 1~7；
Water 1000~50000.
5. a kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material according to claim 1 or 4,
It is characterized in that surfactant described in step 2 is glycidol triethylammonium chloride, N- sodium N-lauroyl sarcosinate, ten
The combination of one or more of six alkyl trimethyl ammonium bromides.
6. a kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material according to claim 1,
It is characterized in that 4 kinds of modified cenosphere in surface described in step 3, titanium source, hydrochloric acid, water components are mixed according to following parts by weight:
7. a kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material according to claim 1,
It is characterized in that titanium source described in step 3 for the combination of one or more of titanium tetrachloride, titanium sulfate, titanyl sulfate.
8. a kind of preparation method of rutile cladding cenosphere infrared external reflection heat-barrier material according to claim 1,
It is characterized in that calcinating system described in step 3 are as follows: be warming up to 200~400 DEG C with 3 DEG C/min and keep the temperature 2~6 hours.
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