CN103864151A - Preparation technology of transparent iron oxide red pigment - Google Patents
Preparation technology of transparent iron oxide red pigment Download PDFInfo
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- CN103864151A CN103864151A CN201210527037.0A CN201210527037A CN103864151A CN 103864151 A CN103864151 A CN 103864151A CN 201210527037 A CN201210527037 A CN 201210527037A CN 103864151 A CN103864151 A CN 103864151A
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Abstract
The invention discloses a preparation technology of a transparent iron oxide red pigment. The preparation technology comprises the following steps of pumping tetraethylene glycol monomethyl ether into a stainless-steel electric-heating reactor by a vacuum pump, carrying out heating to 90 DEG C, feeding transparent iron oxide yellow into the stainless-steel electric-heating reactor according to a weight amount of tetraethylene glycol monomethyl ether to transparent iron oxide yellow of 5: 9 to 3: 5, closely covering a feeding inlet with a cover, carrying out heating, wherein in heating, the transparent iron oxide yellow is in a dehydration state at a reactor interior temperature of 220 DEG C and at the moment, a recovered liquid from a condenser outlet is increased obviously and the temperature of 220 DEG C is automatically kept for about 1.5h until crystallization dehydration is finished and then is automatically increased until the temperature is 250 DEG C, keeping the temperature of 250 DEG C for 1.5h, then stopping heating, simultaneously, increasing the amount of cooling water in a condenser, carrying out vacuum-pumping to pump superfluous tetraethylene glycol methyl ether in the reactor by the vacuum pump, and feeding the superfluous tetraethylene glycol methyl ether into a recovery tank. The transparent iron oxide red pigment has the advantages of high tinting strength, brilliant color and high transparency. The preparation technology has simple processes and low energy consumption.
Description
Technical field
The present invention relates to chemical color field, be specifically related to a kind of preparation technology of the transparent ferric oxide red that is mainly used in the fields such as wood lacquer, automobile finish, metallic paint, building coating, plastics, picture material, high temp glass ink.
Background technology
General transparent ferric oxide red is mainly to be calcined and form in 210 ℃-350 ℃ by transparent yellow iron oxide.Method for cooking mainly contains two kinds: one is to utilize rotary kiln to transparent yellow iron oxide continuous firing; Another kind is to utilize chamber type electric resistance furnace or infrared lamp process furnace intermittently to fire transparent yellow iron oxide.These two kinds of method for cooking exist common shortcoming to be: 1. point for measuring temperature temperature and material actual temperature relative temperature difference are large.2. owing to being all by preset temp, the electric even ﹚ of rear logical thermal overload resistor ﹙ heat controls temperature, large, the wayward grasp of temperature of lower variation of tolerance in design temperature and material actual temperature.3. in sintering procedure, feed intake, when discharging, dust is large.4. in rotary kiln sintering procedure, material is easily tied wall, causes burning not thoroughly or occur sintering phenomenon.5. when chamber type electric resistance furnace or infrared lamp process furnace are fired, heat is inhomogeneous, easily causes upper strata temperature drift sintering, the situations such as end grills thoroughly that lower floor's temperature is on the low side, and the quality of material in same stove is poor easily large, wayward.6. due to these two kinds of method non-uniform temperature, local temperature is too high, makes transparent iron oxide red aberration partially dark, and poor transparency and because of easy-sintering is difficult for disperseing and cause.7. these two kinds of method power consumptions are large simultaneously, and fractional yield is low.
Summary of the invention
The invention provides a kind of tinting strength for the problem existing in background technology high, bright-colored, transparency is high, and the preparation technology of the low transparent ferric oxide red of the simple energy consumption of technique.
The technical solution used in the present invention is as follows: a kind of preparation technology of transparent ferric oxide red, and concrete steps are as follows:
(1) TEG monomethyl ether is utilized vacuum pump pump in stainless steel electric heating reacting kettle, and start heat up heating, in the time that reactor temperature is raised to 90 ℃, open reactor feed mouth, drop into transparent yellow iron oxide, then dog-house is covered tightly and continues to heat up, the weight ratio of the input amount of described TEG monomethyl ether and transparent yellow iron oxide is 5:9 to 3:5;
(2), reclaiming TEG monomethyl ether in condensator outlet access recycling bin, to use while making next time, regulate the flow of water of condensation according to the load that reclaims liquid simultaneously;
(3) in the time that temperature in the kettle arrives 220 ℃, transparent yellow iron oxide enters now condensator outlet recovery of water smoking liquid obviously to be increased, and temperature is automatically in the about 1.5h of this temperature section constant temperature left and right, until exsiccation finishes by Fe
2o
3.H
2o heating generates Fe
2o
3+ H
2o just continues automatic heating, starts insulation timing 1.5h in the time that temperature is raised to 250 ℃;
(4) after timing 1.5h, pass heating increases condenser cooling water amount simultaneously and opens vacuum, utilizes vacuum pump to take out the unnecessary TEG methyl ether in reactor, in accumulator tank, until material stops compared with thickness in groove;
(5) drive vacuum pump, in reactor, slowly add a small amount of water, water add speed control at 3T per hour, water reduces temperature in the kettle, in this process, in still, must keep negative pressure, just can stop below adding water until temperature in the kettle drops to 100 ℃, and stop vacuum pump, open blow-off valve, finally open reactor feed mouth, inwardly rush the cooling of still wall from still mouth;
(6), when temperature in the kettle drops to 90 ℃ of laggard plate-and-frame filter press, with approximately 30 ㎡ water rinses, rinse and be attached to the lip-deep unnecessary TEG monomethyl ether of pigment particles;
(7) go out plate-and-frame filter press, enter steam baking house and dry, pulverize and both obtain ferric oxide red colorant powder.
The preparation technology of a kind of transparent ferric oxide red of the present invention, the TEG monomethyl ether that TEG monomethyl ether in step (1) also can adopt step (2) to reclaim, the TEG monomethyl ether that is about to reclaim utilizes vacuum pump to pump in stainless steel electric heating reacting kettle, and start heat up heating, need be to the condensator outlet emptying of reactor in the time that reactor temperature is raised to 100 ℃ of left and right, the water of now discharging is bled off, in the time that reactor temperature is raised to 120 ℃, it is little that now condensator outlet is discharged liquid measure, opening vacuum pumps to new TEG monomethyl ether in this still, pump TEG monomethyl ether and finish, now temperature is approximately reduced to 90 ℃ of left and right, stops vacuum pump, opens reactor feed mouth, drop into transparent yellow iron oxide, rear dog-house cover tightly continue heat up.
the present inventiona kind of step of preparation process (1) of transparent ferric oxide red described in the weight ratio of input amount of TEG monomethyl ether and transparent yellow iron oxide be 9.5:5.5.
the present inventiona kind of preparation technology of transparent ferric oxide red, described TEG monomethyl ether appearance requirement is as clear as crystal, fluid balance boiling point reflux>=260 ℃.
The present invention has following beneficial effect:
1, constant product quality of the present invention, bright-colored, and gloss is bright, and transparency is high.
2, the transparent iron oxide red unit consumption of energy that utilizes transparent ferric oxide red preparation technology of the present invention to make is low, and relative productivity is high, finishes approximately to use 8h left and right from being dosed into into sheet frame.
3, transparent ferric oxide red preparation technology point for measuring temperature of the present invention is directly with material contact, and temperature control is accurate, is quick on the draw.
4, because transparent ferric oxide red preparation technology of the present invention adopts TEG monomethyl ether, its boiling point reflux temperature is 260 ℃ of left and right, and transparent yellow iron oxide changes into transparent iron oxide red just in time temperature control between 220 ℃-250 ℃, reaching can temperature automatically controlled object.
5, due to transparent ferric oxide red preparation technology of the present invention, be to operate in the container of sealing, work-yard environment is cleaner relatively, has reduced dust.
6, because transparent ferric oxide red preparation technology's of the present invention sintering procedure is to carry out under moisture state, and have and do not stop stirring, so avoided the situation of material knot wall.Make material more even owing to not stopping to stir simultaneously, same batch material steady quality, easy to control.
7, because each point temperature-stable in transparent ferric oxide red preparation technology still of the present invention there will not be local higher phenomenon, material does not produce sintering situation, so the transparent ferric oxide that this kind of method fired more easily disperses.
Embodiment
Below in conjunction with the detailed elaboration the present invention of embodiment.
To be that Jiangsu is happy reach chemical limited-liability company and produce the TEG monomethyl ether of the new-task buying described in embodiment below.Product requirement outward appearance is as clear as crystal, fluid balance boiling point reflux >=260 ℃.Certainly, when reality is used, also can adopt the TEG monomethyl ether with similar quality by other manufacturer production.
Embodiment 1
Prepare a preparation technology for transparent ferric oxide red, its concrete steps are as follows:
Get the TEG monomethyl ether of 900KG new-task buying, utilize vacuum pump to pump in stainless steel electric heating reacting kettle, and start the heating that heats up.When temperature to 90 ℃ left and right, open reactor feed mouth, drop into 500KG transparent yellow iron oxide, then dog-house is covered tightly to follow-up temperature of continuing rising.Under condenser, have two one of outlets to connect recycling bin, one connects accumulator tank.When recycling bin refers to not open vacuum, condensator outlet takes back the bucket of rewinding by valve and flexible pipe, and this bucket can regulate by hose length mobile arbitrarily; When accumulator tank refers to out vacuum, condensator outlet takes back the groove of rewinding, and accumulator tank only uses under vacuum condition, and 1 cube of left and right of this groove is that fixture is irremovable.While using recycling bin, accumulator tank must be closed simultaneously, while using accumulator tank equally, recycling bin must be closed.In above-mentioned intensification, condensator outlet is accessed in recycling bin and reclaims TEG monomethyl ether, use while below producing once, according to the flow of the load adjusting water of condensation of recovery liquid, the flow of water of condensation is generally no more than 40 ℃ according to its water temperature control simultaneously.
In the time that temperature in the kettle arrives 220 ℃, transparent yellow iron oxide enters now condensator outlet recovery of water smoking liquid obviously to be increased, and temperature is automatically in the about 1.5h of this temperature section constant temperature left and right, until exsiccation finishes by Fe
2o
3.H
2o heating generates Fe
2o
3+ H
2o just continues automatic heating.In the time that being raised to 250 ℃, temperature starts insulation timing 1.5h.
After timing 1.5h, close heating and increase condenser cooling water amount simultaneously, 15 tons approximately per hour of the water yield, drive vacuum pump, utilize vacuum pump to take out the unnecessary TEG methyl ether in reactor, close the condensator outlet valve that connects recycling bin simultaneously, condensator outlet is connected to the valve open of accumulator tank, make the unnecessary TEG methyl ether that vacuum is extracted out flow into accumulator tank, until material in reactor stops compared with thickness.Stop vacuum pump, the unnecessary TEG methyl ether pump reclaiming in accumulator tank is pumped in recycling bin.Amount to approximately recyclable TEG methyl ether 900KG left and right.
Drive vacuum pump, in reactor, slowly add a small amount of water, water add speed control at 3T per hour, reduce temperature in the kettle, in this process, in still, must keep negative pressure, just can stop below adding water until temperature in the kettle drops to 100 ℃, and stop vacuum pump, open blow-off valve.Open afterwards again reactor feed mouth, inwardly rush the cooling of still wall from still mouth.
When temperature in the kettle drops to 90 ℃ of laggard plate-and-frame filter press, rinsing.Rinsing water approximately 30 ㎡.Rinse and be attached to the lip-deep unnecessary TEG methyl ether of pigment particles.
Go out plate-and-frame filter press, enter steam baking house and dry, pulverize and both obtain ferric oxide red colorant powder.
Finally check, packing warehouse-in.
Embodiment 2
Prepare a preparation technology for transparent ferric oxide red, its concrete steps are as follows:
Get the TEG monomethyl ether of 1000KG new-task buying, utilize vacuum pump to pump in stainless steel electric heating reacting kettle, and start the heating that heats up.When temperature to 90 ℃ left and right, open reactor feed mouth, drop into 600KG transparent yellow iron oxide, then dog-house is covered tightly to follow-up temperature of continuing rising.Under condenser, have two one of outlets to connect recycling bin, one connects accumulator tank.When recycling bin refers to not open vacuum, condensator outlet takes back the bucket of rewinding by valve and flexible pipe, and this bucket can regulate by hose length mobile arbitrarily; When accumulator tank refers to out vacuum, condensator outlet takes back the groove of rewinding, and accumulator tank only uses under vacuum condition, and 1 cube of left and right of this groove is that fixture is irremovable.While using recycling bin, accumulator tank must be closed simultaneously, while using accumulator tank equally, recycling bin must be closed.In above-mentioned intensification, condensator outlet is accessed in recycling bin and reclaims TEG monomethyl ether, use while below producing once, according to the flow of the load adjusting water of condensation of recovery liquid, the flow of water of condensation is generally no more than 40 ℃ according to its water temperature control simultaneously.
In the time that temperature in the kettle arrives 220 ℃, transparent yellow iron oxide enters now condensator outlet recovery of water smoking liquid obviously to be increased, and temperature is automatically in the about 1.5h of this temperature section constant temperature left and right, until exsiccation finishes by Fe
2o
3.H
2o heating generates Fe
2o
3+ H
2o just continues automatic heating.In the time that being raised to 250 ℃, temperature starts insulation timing 1.5h.
After timing 1.5h, close heating and increase condenser cooling water amount simultaneously, 15 tons approximately per hour of the water yield, drive vacuum pump, utilize vacuum pump to take out the unnecessary TEG methyl ether in reactor, close the condensator outlet valve that connects recycling bin simultaneously, condensator outlet is connected to the valve open of accumulator tank, make the unnecessary TEG methyl ether that vacuum is extracted out flow into accumulator tank, until material in reactor stops compared with thickness.Stop vacuum pump, the unnecessary TEG methyl ether pump reclaiming in accumulator tank is pumped in recycling bin.Amount to approximately recyclable TEG methyl ether 900KG left and right.
Drive vacuum pump, in reactor, slowly add a small amount of water, water add speed control at 3T per hour, reduce temperature in the kettle, in this process, in still, must keep negative pressure, just can stop below adding water until temperature in the kettle drops to 100 ℃, and stop vacuum pump, open blow-off valve.Open afterwards again reactor feed mouth, inwardly rush the cooling of still wall from still mouth.
When temperature in the kettle drops to 90 ℃ of laggard plate-and-frame filter press, rinsing.Rinsing water approximately 30 ㎡.Rinse and be attached to the lip-deep unnecessary TEG methyl ether of pigment particles.
Go out plate-and-frame filter press, enter steam baking house and dry, pulverize and both obtain ferric oxide red colorant powder.
Finally check, packing warehouse-in.
Embodiment 3
Prepare a preparation technology for transparent ferric oxide red, its concrete steps are as follows:
Get the TEG monomethyl ether of 950KG new-task buying, utilize vacuum pump to pump in stainless steel electric heating reacting kettle, and start the heating that heats up.When temperature to 90 ℃ left and right, open reactor feed mouth, drop into 550KG transparent yellow iron oxide, then dog-house is covered tightly to follow-up temperature of continuing rising.Under condenser, have two one of outlets to connect recycling bin, one connects accumulator tank.When recycling bin refers to not open vacuum, condensator outlet takes back the bucket of rewinding by valve and flexible pipe, and this bucket can regulate by hose length mobile arbitrarily; When accumulator tank refers to out vacuum, condensator outlet takes back the groove of rewinding, and accumulator tank only uses under vacuum condition, and 1 cube of left and right of this groove is that fixture is irremovable.While using recycling bin, accumulator tank must be closed simultaneously, while using accumulator tank equally, recycling bin must be closed.In above-mentioned intensification, condensator outlet is accessed in recycling bin and reclaims TEG monomethyl ether, use while below producing once, according to the flow of the load adjusting water of condensation of recovery liquid, the flow of water of condensation is generally no more than 40 ℃ according to its water temperature control simultaneously.
In the time that temperature in the kettle arrives 220 ℃, transparent yellow iron oxide enters now condensator outlet recovery of water smoking liquid obviously to be increased, and temperature is automatically in the about 1.5h of this temperature section constant temperature left and right, until exsiccation finishes by Fe
2o
3.H
2o heating generates Fe
2o
3+ H
2o just continues automatic heating.In the time that being raised to 250 ℃, temperature starts insulation timing 1.5h.
After timing 1.5h, close heating and increase condenser cooling water amount simultaneously, 15 tons approximately per hour of the water yield, drive vacuum pump, utilize vacuum pump to take out the unnecessary TEG methyl ether in reactor, close the condensator outlet valve that connects recycling bin simultaneously, condensator outlet is connected to the valve open of accumulator tank, make the unnecessary TEG methyl ether that vacuum is extracted out flow into accumulator tank, until material in reactor stops compared with thickness.Stop vacuum pump, the unnecessary TEG methyl ether pump reclaiming in accumulator tank is pumped in recycling bin.Amount to approximately recyclable TEG methyl ether 900KG left and right.
Drive vacuum pump, in reactor, slowly add a small amount of water, water add speed control at 3T per hour, reduce temperature in the kettle, in this process, in still, must keep negative pressure, just can stop below adding water until temperature in the kettle drops to 100 ℃, and stop vacuum pump, open blow-off valve.Open afterwards again reactor feed mouth, inwardly rush the cooling of still wall from still mouth.
When temperature in the kettle drops to 90 ℃ of laggard plate-and-frame filter press, rinsing.Rinsing water approximately 30 ㎡.Rinse and be attached to the lip-deep unnecessary TEG methyl ether of pigment particles.
Go out plate-and-frame filter press, enter steam baking house and dry, pulverize and both obtain ferric oxide red colorant powder.
Finally check, packing warehouse-in.
Embodiment 4
Prepare a preparation technology for transparent ferric oxide red, its concrete steps are as follows:
. utilize vacuum pump to pump in stainless steel electric heating reacting kettle the about 800KG of TEG monomethyl ether reclaiming in recycling bin, and start heat up add heat, ﹙ Heating temperature can be transferred to 300 ℃ of ﹚.The TEG monomethyl ether reclaiming in recycling bin described here refers to that the TEG monomethyl ether that in embodiment 1 technique, recycling bin is recovered to reclaims liquid.
(2). in the time that being raised to 100 ℃ of left and right, reactor temperature need, to the condensator outlet emptying of reactor, the water of now discharging be bled off.
(3). in the time that reactor temperature is raised to 120 ℃, it is little that now condensator outlet is discharged liquid measure, and the TEG monomethyl ether that to open vacuum be new-task buying the new TEG monomethyl ether of 100KG pumps in this still.
(4). pump TEG monomethyl ether and finish, now temperature is approximately reduced to 90 ℃ of left and right, stops vacuum pump, opens reactor feed mouth, drops into 500-600KG transparent yellow iron oxide, rear dog-house is covered tightly and continues to heat up.
(5). reclaiming TEG monomethyl ether in condensator outlet access recycling bin, use while below producing once, simultaneously according to the flow of the load adjusting water of condensation of recovery liquid.According to water of condensation water temperature, control is generally no more than 40 ℃ to the flow of water of condensation.
(6). in the time that temperature in the kettle arrives 220 ℃, transparent yellow iron oxide enters now condensator outlet recovery of water smoking liquid obviously to be increased, and temperature is automatically in the about 1.5h of this temperature section constant temperature left and right, until exsiccation finishes by Fe
2o
3.H
2o heating generates Fe
2o
3+ H
2o just continues automatic heating.In the time that being raised to 250 ℃, temperature starts insulation timing 1.5h.
(7). after timing 1.5h, close heating and increase condenser cooling water amount simultaneously, 15 tons approximately per hour of the water yield, drive vacuum pump, utilize vacuum pump to take out the unnecessary TEG methyl ether in reactor, close the condensator outlet valve that connects recycling bin simultaneously, condensator outlet is connected to the valve open of accumulator tank, make the unnecessary TEG methyl ether that vacuum is extracted out flow into accumulator tank, until material in reactor stops compared with thickness.Stop vacuum pump, the unnecessary TEG methyl ether pump reclaiming in accumulator tank is pumped in recycling bin.Amount to approximately recyclable TEG methyl ether 900KG left and right.
(8). drive vacuum pump, in reactor, slowly add a small amount of water, water add speed control at 3T per hour, reduce temperature in the kettle, in this process, in still, must keep negative pressure, just can stop below adding water until temperature in the kettle drops to 100 ℃, and stop vacuum pump, open blow-off valve, then after open reactor feed mouth, inwardly rush still wall cooling from still mouth.
(9). when temperature in the kettle drops to 90 ℃ of laggard plate-and-frame filter press, rinsing.Rinsing water approximately 30 ㎡.Rinse and be attached to the lip-deep unnecessary TEG methyl ether of pigment particles.
(10). go out plate-and-frame filter press, enter steam baking house and dry, pulverize and both obtain ferric oxide red colorant powder.
(11). finally check, packing warehouse-in.
Embodiment 5
Prepare a preparation technology for transparent ferric oxide red, its concrete steps are as follows:
. utilize vacuum pump to pump in stainless steel electric heating reacting kettle the about 800KG of TEG monomethyl ether reclaiming in recycling bin, and start heat up add heat, ﹙ Heating temperature can be transferred to 300 ℃ of ﹚.The TEG monomethyl ether reclaiming in recycling bin described here refers to that the TEG monomethyl ether that in embodiment 1 technique, recycling bin is recovered to reclaims liquid.
(2). in the time that being raised to 100 ℃ of left and right, reactor temperature need, to the condensator outlet emptying of reactor, the water of now discharging be bled off.
(3). in the time that reactor temperature is raised to 120 ℃, it is little that now condensator outlet is discharged liquid measure, and the TEG monomethyl ether that to open vacuum be new-task buying the new TEG monomethyl ether of 200KG pumps in this still.
(4). pump TEG monomethyl ether and finish, now temperature is approximately reduced to 90 ℃ of left and right, stops vacuum pump, opens reactor feed mouth, drops into 600KG transparent yellow iron oxide, rear dog-house is covered tightly and continues to heat up.
(5). reclaiming TEG monomethyl ether in condensator outlet access recycling bin, use while below producing once, simultaneously according to the flow of the load adjusting water of condensation of recovery liquid.According to water of condensation water temperature, control is generally no more than 40 ℃ to the flow of water of condensation.
(6). in the time that temperature in the kettle arrives 220 ℃, transparent yellow iron oxide enters now condensator outlet recovery of water smoking liquid obviously to be increased, and temperature is automatically in the about 1.5h of this temperature section constant temperature left and right, until exsiccation finishes by Fe
2o
3.H
2o heating generates Fe
2o
3+ H
2o just continues automatic heating.In the time that being raised to 250 ℃, temperature starts insulation timing 1.5h.
(7). after timing 1.5h, close heating and increase condenser cooling water amount simultaneously, 15 tons approximately per hour of the water yield, drive vacuum pump, utilize vacuum pump to take out the unnecessary TEG methyl ether in reactor, close the condensator outlet valve that connects recycling bin simultaneously, condensator outlet is connected to the valve open of accumulator tank, make the unnecessary TEG methyl ether that vacuum is extracted out flow into accumulator tank, until material in reactor stops compared with thickness.Stop vacuum pump, the unnecessary TEG methyl ether pump reclaiming in accumulator tank is pumped in recycling bin.Amount to approximately recyclable TEG methyl ether 900KG left and right.
(8). drive vacuum pump, in reactor, slowly add a small amount of water, water add speed control at 3T per hour, reduce temperature in the kettle, in this process, in still, must keep negative pressure, just can stop below adding water until temperature in the kettle drops to 100 ℃, and stop vacuum pump, open blow-off valve, then after open reactor feed mouth, inwardly rush still wall cooling from still mouth.
(9). when temperature in the kettle drops to 90 ℃ of laggard plate-and-frame filter press, rinsing.Rinsing water approximately 30 ㎡.Rinse and be attached to the lip-deep unnecessary TEG methyl ether of pigment particles.
(10). go out plate-and-frame filter press, enter steam baking house and dry, pulverize and both obtain ferric oxide red colorant powder.
(11). finally check, packing warehouse-in.
Finished product proterties detects test:
Same batch of transparent yellow iron oxide for raw material, technique adopts respectively transmission rotary kiln mode and technique of the present invention, and what make is transparent iron oxide red.Then detect by coating method transparent iron oxide red the product obtaining respectively.Detection method is as follows:
1, prepare base-material:
Long oil alkyd (389-8) 140g
200# solvent oil 120g
BYK-106 dispersion agent 30g
2, system slurry in vain:
Base-material 58g
Rutile type Titanium Dioxide 42g
Zirconium pearl (￠ 1.0-1.6 ㎜) 150g
Be placed in 125ml vial grinds 1hr and obtains white slurry on automatic mixing machine.
3, mill base processed:
(1), standard specimen (rotary kiln technology)
Base-material 40.6g
The transparent iron oxide red 20g that rotary kiln technology makes
Zirconium pearl (￠ 1.0-1.6 ㎜) 220g
(2), sample (technique of the present invention)
Base-material 40.6g
The transparent iron oxide red 20g that technique of the present invention makes
Zirconium pearl (￠ 1.0-1.6 ㎜) 220g
Be placed in respectively 125ml vial simultaneous grinding 1hr on same automatic mixing machine and obtain mill base.
4, transparency comparison:
Get mill base 2g, add long oil alkyd 6g fully to stir evenly, standard specimen and sample operate equally.Get and stir evenly slurry and be placed on same black and white paper card, by 100um Wound-rotor type paint film spreader masking.Colorimetric under standard light source, in black matrix, color depth person is that transparency is good.
5, reduced tint comparison:
Get 0.4g mill base, the white slurry of 6.82g fully stirs evenly.Standard specimen and sample operate equally.Get and stir evenly slurry and be placed on same black and white paper card, by 100um Wound-rotor type paint film spreader masking, dry rear by data color 300 color measurement instruments mensuration color parameter and tinting strengths.
6, detected result is as follows:
△ L brightness 1.63
△ a (red green) 0.92
△ b (Huang Lan) 1.25
△ c (variegated) 1.20
Tinting strength 98.75
Transparency is obviously high
Conclusion: can learn according to above-mentioned detected result, the pigment ratio that utilizes technique of the present invention to prepare is brighter, form and aspect orange, saturation ratio is high, and tinting strength is basic identical with the product making with rotary kiln technology.
Claims (4)
1. a preparation technology for transparent ferric oxide red, is characterized in that: concrete steps are as follows:
(1) TEG monomethyl ether is utilized vacuum pump pump in stainless steel electric heating reacting kettle, and start heat up heating, in the time that reactor temperature is raised to 90 ℃, open reactor feed mouth, drop into transparent yellow iron oxide, then dog-house is covered tightly and continues to heat up, the weight ratio of the input amount of described TEG monomethyl ether and transparent yellow iron oxide is 5:9 to 3:5;
(2), reclaiming TEG monomethyl ether in condensator outlet access recycling bin, to use while making next time, regulate the flow of water of condensation according to the load that reclaims liquid simultaneously;
(3) in the time that temperature in the kettle arrives 220 ℃, transparent yellow iron oxide enters now condensator outlet recovery of water smoking liquid obviously to be increased, and temperature is automatically in the about 1.5h of this temperature section constant temperature left and right, until exsiccation finishes by Fe
2o
3.H
2o heating generates Fe
2o
3+ H
2o just continues automatic heating, starts insulation timing 1.5h in the time that temperature is raised to 250 ℃;
(4) after timing 1.5h, pass heating increases condenser cooling water amount simultaneously and opens vacuum, utilizes vacuum pump to take out the unnecessary TEG methyl ether in reactor, in accumulator tank, until material stops compared with thickness in groove;
(5) drive vacuum pump, in reactor, slowly add a small amount of water, water add speed control at 3T per hour, water reduces temperature in the kettle, in this process, in still, must keep negative pressure, just can stop below adding water until temperature in the kettle drops to 100 ℃, and stop vacuum pump, open blow-off valve, finally open reactor feed mouth, inwardly rush the cooling of still wall from still mouth;
(6), when temperature in the kettle drops to 90 ℃ of laggard plate-and-frame filter press, with approximately 30 ㎡ water rinses, rinse and be attached to the lip-deep unnecessary TEG monomethyl ether of pigment particles;
(7) go out plate-and-frame filter press, enter steam baking house and dry, pulverize and both obtain ferric oxide red colorant powder.
2. the preparation technology of a kind of transparent ferric oxide red as claimed in claim 1, it is characterized in that: the TEG monomethyl ether that the TEG monomethyl ether in step (1) also can adopt step (2) to reclaim, the TEG monomethyl ether that is about to reclaim utilizes vacuum pump to pump in stainless steel electric heating reacting kettle, and start heat up heating, need be to the condensator outlet emptying of reactor in the time that reactor temperature is raised to 100 ℃ of left and right, the water of now discharging is bled off, in the time that reactor temperature is raised to 120 ℃, it is little that now condensator outlet is discharged liquid measure, opening vacuum pumps to new TEG monomethyl ether in this still, pump TEG monomethyl ether and finish, now temperature is approximately reduced to 90 ℃ of left and right, stops vacuum pump, opens reactor feed mouth, drop into transparent yellow iron oxide, rear dog-house cover tightly continue heat up.
3. the preparation technology of a kind of transparent ferric oxide red as claimed in claim 1, is characterized in that: described in step (1), the weight ratio of the input amount of TEG monomethyl ether and transparent yellow iron oxide is 9.5:5.5.
4. the preparation technology of a kind of transparent ferric oxide red as described in claim 1 or 2 or 3, is characterized in that: described TEG monomethyl ether appearance requirement is as clear as crystal, fluid balance boiling point reflux >=260 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4618375A (en) * | 1984-10-04 | 1986-10-21 | Basf Corporation | Transparent iron oxide pigments |
| CN102295313A (en) * | 2008-01-09 | 2011-12-28 | 麦格霍斯奈米生技股份有限公司 | Magnetic transducers |
-
2012
- 2012-12-10 CN CN201210527037.0A patent/CN103864151B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4618375A (en) * | 1984-10-04 | 1986-10-21 | Basf Corporation | Transparent iron oxide pigments |
| CN102295313A (en) * | 2008-01-09 | 2011-12-28 | 麦格霍斯奈米生技股份有限公司 | Magnetic transducers |
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