CN106219611B - A kind of low viscosity iron oxide yellow - Google Patents
A kind of low viscosity iron oxide yellow Download PDFInfo
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- CN106219611B CN106219611B CN201610596145.1A CN201610596145A CN106219611B CN 106219611 B CN106219611 B CN 106219611B CN 201610596145 A CN201610596145 A CN 201610596145A CN 106219611 B CN106219611 B CN 106219611B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
Abstract
The invention discloses a kind of low viscosity iron oxide yellow, the method that the iron oxide yellow is used is that reaction prepares iron oxide yellow crystal seed under the conditions of 25 35 DEG C by ferrous sulfate and NaOH, then the crystal seed prepared is put into autoclave, temperature is risen to 70 DEG C simultaneously, now air pressure is identical with the external world in reactor, when temperature reaches 70 DEG C, add the sodium hydroxide solution that concentration is 8 12mol/L, the liquid caustic soda amount of addition is defined by pH value, stop adding liquid caustic soda when pH reaches 3.8 4.2, autoclave valve is closed after defined pH is reached, and autoclave is pressurizeed by pressure-air pump, constantly air is squeezed into course of reaction from reactor bottom with high-pressure pump, gas is released at the top of reactor simultaneously, to ensure that sufficient oxygen participates in reaction, control system air pressure is in 1.2 1.7MPa air pressure or so, reaction temperature is 70 DEG C.Low viscosity iron oxide yellow is made finally by rinsing, suction filtration, drying, crushing in 12 14h in reaction time control.
Description
Technical field
The present invention relates to a kind of low viscosity ferric oxide yellow pigment, and in particular to by controlling pressure in course of reaction, pH
The conditions such as value, temperature, reaction time prepare low viscosity iron oxide yellow.
Technical background
Iron oxide yellow, also known as FeOOH, its molecular formula are FeOOH or Fe2O3H2O, in yellow powder, its grain
Son is shaped as needle-like, with higher tinting strength, tinting power, covering power, and nontoxic, is environmentally friendly inorganic pigment, its light resistance
Reach 6-7 grades.Ferric oxide yellow pigment is widely used in building materials, coating, paint, plastics, rubber, electronics, industrial catalyst, cigarette
The industries such as grass, cosmetics.
Common iron oxide yellow is different with surface chemistry due to particle shape, and its viscosity is higher, in coating application process
It is middle to there are problems that, it is spherical with other isometric systems such as iron oxide red, iron oxide black is compared for cube, iron oxide yellow
It is acicular texture, and the length-width ratio of its aciculiform is different.Because needle-like structures, cause iron oxide yellow and the iron oxide of isometric system
It is red to be compared with iron oxide black, with higher resistance to flow energy, so its viscosity highest in the coating system of most of media,
The problem of being also the maximum that coating and pigment industry are run into.
The rheological property of coating, from construction to film forming, all has strict demand, at this from beginning to end from production to storage
In a little stages, because the concentration of pigment is different, the shearing force that coating is subjected to is different with pressure, so viscosity or resistance to flow can be
One key technical index of coating, in the grinding stage of high shear force, in order that pigment content reaches peak in mill base, to the greatest extent
Amount improves production efficiency, it is desirable to which the viscosity for grinding base is lower, and its viscosity also is intended in the mixing of coating, transfer, packaging process
It is lower.
The all components of coating all have a certain impact to viscosity, and for the viscosity characteristicses required by acquisition, selection is suitable
Pigment is a key factor.The important development direction for being coating industry at present with high solids low volatile organic, and face
The viscosity of material determines the size of solid content, and pigment viscosity is too high, causes coating resistance to flow higher, totally unfavorable to producing.
There is ' one kind reduction oxidation of the Nantong Bao Ju pigment company issued patents number for ZL201310277999.X the current country
The method of iron oxide yellow pigments viscosity ' patent and authorized.Zhejiang joint pigment discloses the special of application number 201410767118.7
Sharp " a kind of low viscosity ferric oxide yellow pigment ".The patent that Chou Xuekang discloses Application No. 201510161430.6 is " a kind of low viscous
Spend ferric oxide yellow pigment ".
At present, domestic and international pertinent literature report display, is aoxidized by changing iron oxide yellow particle surface electric charge or reducing
The draw ratio of iron oxide yellow particle can be improved to the viscosity of iron oxide yellow, and there are Nantong Bao Ju pigment company issued patents the country
Number for ZL201310277999.X the method for ferric oxide yellow pigment viscosity ' a kind of reduce ' patent i.e. by changing iron oxide yellow
The electric charge of particle surface improves the viscosity of iron oxide yellow, and effect is more satisfactory, but still have improved space;And Zhejiang joint face
A kind of patent " low viscosity ferric oxide yellow pigment " of the disclosed application number 201410767118.7 of material, its principle is by steel
Pearl is ground, and destroys partial oxidation iron oxide yellow pigments shape of particle, and can not reduce the draw ratio of all iron oxide yellow particles on the whole,
Its effect is not notable enough.
The content of the invention
The present invention in view of the shortcomings of the prior art, it is an object of the invention to provide a kind of low viscosity iron oxide yellow preparation method,
This method, by changing reaction environment, reduces iron oxide yellow face under conditions of being added without other materials and changing pigment pH value
Expect viscosity.
In order to realize above-mentioned purpose, present invention employs following technical scheme:
A kind of low viscosity iron oxide yellow, the preparation method of the iron oxide yellow comprises the following steps:
1)It is prepared by crystal seed:
A:Raw material is configured:Concentration is added in stainless steel reaction bucket for 1.0mol/L-2.0mol/L copperas solution,
It is 1/3 copperas solution volume, the sodium hydroxide solution that concentration is 8-12mol/L to add volume, while controlling reaction
Temperature is 25-35 DEG C;
B:Boiler pressure control:It is 14-17h to control total reaction time, and first 5-7 hours is passed through air to reaction solution bottom, empty
Tolerance is controlled in 230L/h, and rear 7-10h is passed through air to reaction solution bottom, and air capacity is controlled in 460L/h.React final material
Storage is individually laid in as crystal seed;
2)High-pressure oxidation:
A:The crystal seed prepared is put into autoclave, while heated to reactor, temperature control at 70 DEG C, this
When reactor in air pressure it is identical with the external world;
B:When temperature reaches 70 DEG C, the sodium hydroxide solution that concentration is 8-12mol/L is added, the liquid caustic soda amount of addition is with pH
Value is defined, and stops adding liquid caustic soda when pH reaches 3.8-4.2;
C:Autoclave valve is closed after defined pH is reached, and autoclave is carried out by pressure-air pump
Air constantly is squeezed into from reactor bottom with high-pressure pump in pressurization, course of reaction, while gas is released at the top of reactor, to protect
The sufficient oxygen of card participates in reaction, and control system air pressure is in 1.2-1.7MPa air pressure, and reaction temperature is 70 DEG C, reaction time control
In 12-14h;
3)Road is handled afterwards
A:Reaction was reached after the stipulated time, opened reactor valve, released feed liquid, and suction filtration, rinsing are carried out to feed liquid, is dried
Dry, ultra-fine grinding is got product.
As a further improvement, described reactor includes kettle, kettle cover and the reactor outer layer containing heating wire, kettle
It is connected with kettle cover by flange, autoclave body bottom sets baiting valve;It is characterized in that:PH is provided with kettle cover and automatically controls dress
Put, electronic high voltage liquid caustic soda charging valve, high pressure crystal seed charging valve, temperature indicating device, high pressure admission valve, pressure gauge and automatic exhaust
Valve;PH automatons include pH displays and pH determines probe, and pH displays are arranged on the outside of kettle cover, and pH determines probe and set
Put in autoclave body bottom, pH automatons connection control electronic high voltage liquid caustic soda charging valve is being determined after pH reaches setting pH certainly
It is dynamic to close electronic high voltage liquid caustic soda charging valve;Temperature indicating device includes temp probe, and temp probe is arranged on autoclave body bottom;High pressure
Intake valve is connected with air hose, and air hose extends to autoclave body bottom, high pressure admission valve by outside air squeeze into kettle with
For the oxygen needed for reaction, reactor off-gas is discharged outside kettle by automatic exhaust steam valve, then high pressure admission valve again will be extraneous empty
Gas is squeezed into kettle, is circulated successively, it is ensured that oxygen content and pressure value in kettle.
Preferably, described air hose includes being provided with gas outlet on the comb for being arranged on autoclave body bottom, comb.
The effect that the present invention is reached:Reaction under high pressure environment prepares iron oxide yellow, is being added without any auxiliary substance and not
In the case of changing pH value in reaction, low viscosity iron oxide yellow is obtained, the viscosity of product is substantially reduced, be more suitable for various coating colors
The preparation of slurry, adds value-added content of product, has widened application field, is that enterprise adds economic benefit.
Brief description of the drawings
Fig. 1 is structural representation of the invention.
Embodiment
One kind as shown in Figure 1 prepares low draw ratio iron oxide yellow special high-pressure reactor, the reactor include kettle 12,
Kettle cover 13 and the reactor outer layer containing heating wire 8, kettle 12 are connected with kettle cover 13 by flange, and the bottom of kettle 12 sets and put
Expect valve 14;PH automatons 1, electronic high voltage liquid caustic soda charging valve 2, high pressure crystal seed charging valve 3, temperature are provided with kettle cover 13
Instruction device 4, high pressure admission valve 5, pressure gauge 6 and automatic exhaust steam valve 7;PH automatons 1 include pH displays and pH is surveyed
Surely 9, pH displays of popping one's head in are arranged on the outside of kettle cover 13, and pH determines probe 9 and is arranged on the bottom of kettle 12, pH automatons 1
Connection control electronic high voltage liquid caustic soda charging valve 2, electronic high voltage liquid caustic soda charging valve 2 is closed determining after pH reaches setting pH automatically;
Temperature indicating device 4 includes temp probe 10, and temp probe 10 is arranged on the bottom of kettle 12;High pressure admission valve 5 is connected with
Air hose 11, air hose 11 extends to the bottom of kettle 12, and air hose 11 includes setting on the comb for being arranged on the bottom of kettle 12, comb
It is equipped with gas outlet.High pressure admission valve 5 squeezes into outside air in kettle 12 for the oxygen needed for reaction, passes through automatic exhaust steam valve
7 discharge reactor off-gas outside kettle 12, and then high pressure admission valve 5 again squeezes into outside air in kettle 12, circulates successively, it is ensured that
Oxygen content and pressure value in kettle 12.
The function of each part of the present invention is as follows:
A:Include heater heating wire 8 on kettle, kettle 12 can be electrically heated, surveyed on kettle 12 equipped with temperature
Determine instrument, temperature-indicating instrument includes temperature and indicates 4 and temperature-sensing probe 10, can be accurate when being reacted solution reaction kettle
Interior temperature, is normally carried out to react.
B:Include pH automatons 1 on kettle 12, it is determined probe 9 and constituted by pH displays, pH, and wherein pH is determined
Instrument is connected with electronic high voltage liquid caustic soda charging valve 2, automatic after setting pH is reached to close charging valve, due to for reaction its to pH
Control require it is higher, so pH automatons for reaction be normally carried out hold the balance.
C:Include the device that gas reactor is reacted in automatic pressure-controlled, automatic replacing on kettle 12, it is pressed into by pressure gauge 6, height
Air valve 5, automatic exhaust valve 7, as the oxygen needed for high pressure admission valve 5 squeezes into outside air in kettle 12 for reaction, lead to
Cross automatic exhaust steam valve 7 to discharge reactor off-gas outside kettle 12, now high pressure admission valve again squeezes into outside air in kettle 12, according to
Secondary circulation, it is ensured that oxygen content and pressure value in kettle 12, to ensure being normally carried out for reaction.
D:Kettle 12 includes high-pressure crystal seed charging valve 3, can squeeze into crystal seed inside kettle 12.
E:Kettle 12 includes baiting valve, passes through baiting valve blowing after completion of the reaction.
Embodiment 1
1. it is prepared by crystal seed:8L concentration is added in 30L stainless steel reactions bucket for 1.5mol/L copperas solution, added
Enter 10mol/L sodium hydroxide solution 2.5L, while controlling reaction temperature is 30 DEG C.It is 15h, preceding 5- to control total reaction time
Air is passed through within 7 hours to reaction solution bottom, air capacity is controlled in 230L/h, and rear 7-10h is passed through air, air to reaction solution bottom
Amount control is in 460L/h.
2. reaction under high pressure:The 10L crystal seeds prepared are put into autoclave, while being heated to reactor, temperature
Control, at 70 DEG C, is now 1 atmospheric pressure in reactor, when temperature reaches 70 DEG C, adds the hydroxide that concentration is 10mol/L
Sodium solution, the liquid caustic soda amount of addition is defined by pH value, stops adding liquid caustic soda when pH reaches 4.0.Closed after defined pH is reached
Autoclave valve, and autoclave is pressurizeed by pressure-air pump, constantly from reactor bottom in course of reaction
Portion squeezes into air with high-pressure pump, while gas is released at the top of reactor, to ensure that the oxygen of abundance participates in reacting, control system
Air pressure is in 1.2MPa air pressure or so, and reaction temperature is 70 DEG C.Reaction time is controlled in 12h.
3. after road handle:Reaction was reached after the stipulated time, opened reactor valve, releases feed liquid, feed liquid is taken out
Filter, rinsing, drying, ultra-fine grinding get product A.
Embodiment 2
1. it is prepared by crystal seed:8L concentration is added in 30L stainless steel reactions bucket for 1.5mol/L copperas solution, added
Enter 10mol/L sodium hydroxide solution 2.5L, while controlling reaction temperature is 30 DEG C.It is 15h, preceding 5- to control total reaction time
Air is passed through within 7 hours to reaction solution bottom, air capacity is controlled in 230L/h, and rear 7-10h is passed through air, air to reaction solution bottom
Amount control is in 460L/h.
2. reaction under high pressure:The 10L crystal seeds prepared are put into autoclave, while being heated to reactor, temperature
Control, at 70 DEG C, is now 1 atmospheric pressure in reactor, when temperature reaches 70 DEG C, adds the hydroxide that concentration is 10mol/L
Sodium solution, the liquid caustic soda amount of addition is defined by pH value, stops adding liquid caustic soda when pH reaches 4.0.Closed after defined pH is reached
Autoclave valve, and autoclave is pressurizeed by pressure-air pump, constantly from reactor bottom in course of reaction
Portion squeezes into air with high-pressure pump, while gas is released at the top of reactor, to ensure that the oxygen of abundance participates in reacting, control system
Air pressure is in 1.4MPa air pressure or so, and reaction temperature is 70 DEG C.Reaction time is controlled in 12h.
3. after road handle:Reaction was reached after the stipulated time, opened reactor valve, releases feed liquid, feed liquid is taken out
Filter, rinsing, drying, ultra-fine grinding get product B.
Embodiment 3
1. it is prepared by crystal seed:8L concentration is added in 30L stainless steel reactions bucket for 1.5mol/L copperas solution, added
Enter 10mol/L sodium hydroxide solution 2.5L, while controlling reaction temperature is 30 DEG C.It is 15h, preceding 5- to control total reaction time
Air is passed through within 7 hours to reaction solution bottom, air capacity is controlled in 230L/h, and rear 7-10h is passed through air, air to reaction solution bottom
Amount control is in 460L/h.
2. reaction under high pressure:The 10L crystal seeds prepared are put into autoclave, while being heated to reactor, temperature
Control, at 70 DEG C, is now 1 atmospheric pressure in reactor, when temperature reaches 70 DEG C, adds the hydroxide that concentration is 10mol/L
Sodium solution, the liquid caustic soda amount of addition is defined by pH value, stops adding liquid caustic soda when pH reaches 4.0.Closed after defined pH is reached
Autoclave valve, and autoclave is pressurizeed by pressure-air pump, constantly from reactor bottom in course of reaction
Portion squeezes into air with high-pressure pump, while gas is released at the top of reactor, to ensure that the oxygen of abundance participates in reacting, control system
Air pressure is in 1.6MPa air pressure or so, and reaction temperature is 70 DEG C.Reaction time is controlled in 12h.
3. after road handle:Reaction was reached after the stipulated time, opened reactor valve, releases feed liquid, feed liquid is taken out
Filter, rinsing, drying, ultra-fine grinding get product C.
Embodiment 4
1. it is prepared by crystal seed:8L concentration is added in 30L stainless steel reactions bucket for 1.5mol/L copperas solution, added
Enter 10mol/L sodium hydroxide solution 2.5L, while controlling reaction temperature is 30 DEG C.It is 15h, preceding 5- to control total reaction time
Air is passed through within 7 hours to reaction solution bottom, air capacity is controlled in 230L/h, and rear 7-10h is passed through air, air to reaction solution bottom
Amount control is in 460L/h.
2. reaction under high pressure:The 10L crystal seeds prepared are put into autoclave, while being heated to reactor, temperature
Control, at 70 DEG C, is now 1 atmospheric pressure in reactor, when temperature reaches 70 DEG C, adds the hydroxide that concentration is 10mol/L
Sodium solution, the liquid caustic soda amount of addition is defined by pH value, stops adding liquid caustic soda when pH reaches 4.0.Closed after defined pH is reached
Autoclave valve, and autoclave is pressurizeed by pressure-air pump, constantly from reactor bottom in course of reaction
Portion squeezes into air with high-pressure pump, while gas is released at the top of reactor, to ensure that the oxygen of abundance participates in reacting, control system
Air pressure is in 1.4MPa air pressure or so, and reaction temperature is 70 DEG C.Reaction time is controlled in 14h.
3. after road handle:Reaction was reached after the stipulated time, opened reactor valve, releases feed liquid, feed liquid is taken out
Filter, rinsing, drying, ultra-fine grinding get product D.
Embodiment 5
1. it is prepared by crystal seed:8L concentration is added in 30L stainless steel reactions bucket for 1.5mol/L copperas solution, added
Enter 10mol/L sodium hydroxide solution 2.5L, while controlling reaction temperature is 30 DEG C.It is 15h, preceding 5- to control total reaction time
Air is passed through within 7 hours to reaction solution bottom, air capacity is controlled in 230L/h, and rear 7-10h is passed through air, air to reaction solution bottom
Amount control is in 460L/h.
2. reaction under high pressure:The 10L crystal seeds prepared are put into autoclave, while being heated to reactor, temperature
Control, at 70 DEG C, is now 1 atmospheric pressure in reactor, when temperature reaches 70 DEG C, adds the hydroxide that concentration is 10mol/L
Sodium solution, the liquid caustic soda amount of addition is defined by pH value, stops adding liquid caustic soda when pH reaches 4.0.Closed after defined pH is reached
Autoclave valve, and autoclave is pressurizeed by pressure-air pump, constantly from reactor bottom in course of reaction
Portion squeezes into air with high-pressure pump, while gas is released at the top of reactor, to ensure that the oxygen of abundance participates in reacting, control system
Air pressure is in 1.4MPa air pressure or so, and reaction temperature is 70 DEG C.Reaction time is controlled in 16h.
3. after road handle:Reaction was reached after the stipulated time, opened reactor valve, releases feed liquid, feed liquid is taken out
Filter, rinsing, drying, ultra-fine grinding get product E.
Viscosimetric analysis is carried out to the paint mill base of identical solid content using stormer viscosity meter, is ensureing every oil determined
The viscosity number that every experimental product is measured in the case of the solid content identical for painting mill base is as shown in the table:
Remarks:Find that reduction of the reaction time to viscosity has no outstanding role after by many experiments, and reaction pressure
Reduction of the power to viscosity has conclusive effect.The experimental product of common process is with its viscosity number of the paint mill base of prescribed formula
For 125KU, and the paint mill base of the gained experimental product prescribed formula of embodiment 5 its viscosity number is 44-45KU.Reach common
1/3 or so of technique iron oxide yellow viscosity number.
Claims (1)
1. a kind of preparation method of low viscosity iron oxide yellow, it is characterised in that the iron oxide yellow is prepared into using following method
Arrive:
1)It is prepared by crystal seed:8L concentration is added in 30L stainless steel reactions bucket for 1.5mol/L copperas solution, added
10mol/L sodium hydroxide solution 2.5L, while controlling reaction temperature is 30 DEG C;It is 15h, preceding 5-7 to control total reaction time
Hour is passed through air to reaction solution bottom, and air capacity is controlled in 230L/h, and rear 7-10h is passed through air, air to reaction solution bottom
Amount control is in 460L/h;
2)Reaction under high pressure:The 10L crystal seeds prepared are put into autoclave, while being heated to reactor, temperature control
At 70 DEG C, it is now 1 atmospheric pressure in reactor, when temperature reaches 70 DEG C, adds concentration molten for 10mol/L NaOH
Liquid, the liquid caustic soda amount of addition is defined by pH value, stops adding liquid caustic soda when pH reaches 4.0;High pressure is closed after defined pH is reached
Reactor valve, and autoclave is pressurizeed by pressure-air pump, constantly used in course of reaction from reactor bottom
High-pressure pump squeezes into air, while gas is released at the top of reactor, to ensure that the oxygen of abundance participates in reacting, control system air pressure
In 1.2MPa air pressure, reaction temperature is 70 DEG C;Reaction time is controlled in 12h;
3)Road is handled afterwards:Reaction was reached after the stipulated time, opened reactor valve, released feed liquid, and suction filtration, drift are carried out to feed liquid
Wash, dry, ultra-fine grinding is got product.
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CN110342583B (en) * | 2019-07-02 | 2021-07-13 | 浙江华源颜料股份有限公司 | Method for controlling viscosity of iron oxide yellow by using amino acid crystal form control agent |
CN110217826A (en) * | 2019-07-02 | 2019-09-10 | 浙江华源颜料股份有限公司 | A kind of preparation method of the low viscosity iron oxide yellow of microwave intervention |
CN110255624B (en) * | 2019-07-02 | 2021-12-21 | 浙江华源颜料股份有限公司 | Method for controlling viscosity of iron oxide yellow by buffer system |
CN111874955A (en) * | 2020-07-22 | 2020-11-03 | 浙江华源颜料股份有限公司 | Preparation method of iron oxide yellow with high specific surface area |
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