CN108047769A - The method for reducing di-iron trioxide viscosity - Google Patents
The method for reducing di-iron trioxide viscosity Download PDFInfo
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- CN108047769A CN108047769A CN201711389688.7A CN201711389688A CN108047769A CN 108047769 A CN108047769 A CN 108047769A CN 201711389688 A CN201711389688 A CN 201711389688A CN 108047769 A CN108047769 A CN 108047769A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/22—Compounds of iron
- C09C1/24—Oxides of iron
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/043—Drying, calcination
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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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
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Abstract
The invention discloses the methods for reducing di-iron trioxide viscosity, technical grade di-iron trioxide filter cake material is carried out plus water mashing is scattered, above-mentioned di-iron trioxide and water are added in reaction container and form 70~85 DEG C slurries that concentration is 10~14%, control of temperature, then it is 9.0~9.5 to add in lye and control material liquid PH value, when high-speed stirred 3.5~4 is small.This method is simple and convenient, and being not added with any metal ion or oxide just can quickly reduce di-iron trioxide, and di-iron trioxide viscosity can reduce by 30~34KU.
Description
Technical field
The present invention relates to the processing methods of di-iron trioxide, and in particular to by controlling certain slurry concentration, pH value, temperature
The method that degree, mixing speed and mixing time reduce di-iron trioxide viscosity.
Background technology
Di-iron trioxide is also known as iron carbonyl abbreviation iron oxide yellow, is the more stable oxide of chemical property.Chemical molecular formula is
Fe2O3·H2O or FeOOH, in yellow powder.Color and luster has a system from lemon yellow to orange with distinct pure ochre yellow
Row coloured light.It is the aquo-compound of aciculiform, strong covering power, tinting strength, tinting power are high, nontoxic, light resistance up to 6~7 grades, insoluble in alkali, micro-
It is dissolved in acid.Di-iron trioxide is widely used in building materials, coating, paint, plastics, rubber, electronic material, industrial catalyst, tobacco, change
The industries such as cosmetic.
Industrially, most producers domestic at present prepare di-iron trioxide using iron plate method technique, and only several producers use
Liquid phase method technique prepares di-iron trioxide.It traces it to its cause：Iron plate method technics comparing is ripe, and advantage is that pH value is to lean in reaction process
It maintains to stablize automatically after system internal-response, additional need not control, product colour is controllably stablized relatively；Shortcoming is the reaction time
It is long, generally require 2~3 days, iron plate is into bucket and clear bucket be cumbersome, labor intensity is big, in addition iron filings and impurity in final products
Content is high.
And liquid phase method technique provides the new production method of production di-iron trioxide, only needs crystal seed, ferrous iron, alkali；Production week
Time phase is short (20~30 hour or so)；Clear bucket is not required, into iron plate, so as to reduce work personnel, reduce work load
And production cost；We have overcome the uppity deficiency of pH value in reaction process at present, again such that liquid phase method technique system
Standby di-iron trioxide particle diameter is uniform, and external colour index, dispersiveness and other physical properties and iron plate technique are one
Sample, and liquid phase method iron oxide yellow product purity and residue on sieve index are better than iron plate method iron oxide yellow.Further, since this technique does not select scrap iron
Piece can greatly reduce content of beary metal, improve products application performance, the purposes of extended products.
Above two production technology is as follows：
Iron plate method iron oxide yellow production technology：Under the conditions of 25~40 DEG C of temperature, first generated with liquid caustic soda part neutralisation of sulphuric acid is ferrous
Ferrous hydroxide prepares crystal seed with air oxidation ferrous hydroxide, then sub- with air oxidation sulfuric acid in the presence of crystal seed, iron plate
Iron (80~85 DEG C of oxidizing temperature), makes Fe2+It is deposited on the oxygen effect generation ferric iron in air on crystal seed, while the sulphur being precipitated
Acid generates new FeSO with iron sheet effect again4, such constantly circular response promotes seed particles to grow up, gradually forms hydration
Iron oxide (i.e. di-iron trioxide), by the way that three oxygen from light color to a series of dark form and aspect can be obtained to the control that coloured light is in progress
Change two iron pigment.
Liquid phase method iron oxide yellow production technology：It is ferrous with liquid caustic soda (or ammonia) part neutralisation of sulphuric acid under the conditions of 25~40 DEG C of temperature
Ferrous hydroxide is generated, crystal seed is prepared with air oxidation ferrous hydroxide, air oxidation ferrous sulfate (oxygen is used in the presence of crystal seed
Change 80~85 DEG C of temperature), ferrous sulfate and alkali (or ammonia) is continuously added dropwise in reaction process, keeps certain ferrous iron concentration and pH value
(PH=2.5~3.5), by the way that the di-iron trioxide from light color to a series of dark form and aspect can be obtained to the control that coloured light is in progress
Pigment.
Known by above-mentioned iron oxide yellow production technology, industrial di-iron trioxide pigment be slant acidity system (PH=2.5~
3.5) being prepared in, pigment particles itself can adsorb or carry secretly some fine particles and acidic liquid, though through filter-press water-washing
Afterwards, most of fine particle and acidic liquid can wash away, and pH value can slightly rise (PH=3.5~4.5), but in iron oxide yellow pigments
It can also be there are a small amount of small particles and acidic liquid, along with the mutual reunion between pigment particles and particle its own face are thick
The factors such as rough, rough so that iron oxide particles show larger resistance to flow energy, so that technical grade di-iron trioxide
Viscosity number it is generally higher.
The importance of viscosity：
Rheology (or flowing) performance of coating is all to have strictly from beginning to end from construction to film forming from production to storage
It asks.In these stages, since pigment volume concentration (PVC) (PVC) is different, the pressure and shearing that coating is subjected to are also different.Therefore, glue
Resistance to flow energy in other words is spent, is a key index of all types coating, under normal circumstances, in the grinding rank of high shear force
Section, in order to which pigment content in mill base is made to reach peak, improves production efficiency, it is desirable to which the viscosity for grinding base is more relatively low as far as possible.It is applying
In the mixing of material, transfer and packaging process, viscosity also requires lower.
Di-iron trioxide is always for coatings enterprises formulator since particle shape and surface chemistry are different
The maximum of viscosity problem is because of difficulty.Different from other isometric systems (spherical or cube) type, di-iron trioxide is needle-shaped crystal form,
Its aciculiform length-width ratio is also different, this just determines its appearance Huang phase degree.Because it is needle-shaped crystal form, di-iron trioxide particle
Larger resistance to flow energy is showed than most of spherical iron oxide particles, so in most of coating system medium viscosities naturally also
It is high.This is determined by the particle shape of di-iron trioxide.
The all components of coating all have an impact viscosity, to obtain required viscosity characteristics, suitable pigment are selected to be
One crucial factor.As to the solid part of height, the direction of low VOC (VOC) coating is developed, is caused to new
The demand (including iron oxide) of pigment, makes designer have greater flexibility in component design.Therefore, viscosity it is relatively low three
Aoxidizing two iron pigment helps to meet this demand.
Though foreign countries have been reported the di-iron trioxide pigment of low viscosity characteristics：Such as the George Podolsky (U.S. of the U.S.
Extra large Coase pigment company) at home " coatings industry " the 4th phase in 1997 publish thesis summary it is as follows：To di-iron trioxide and other
The understanding of iron oxide difference generates the method for solving high viscosity puzzlement, and there are two possible approach:Change the shape of particle, change
Become the surface charge of particle.It reduces di-iron trioxide acicular particles and waits what shape shafts were possible to close.This can be by making
Particle growth state is realized as improved treatment during standby.But this method there are one it is potential the problem of, i.e. shape of particle
Influence the color of pigment.And when preparing straight-shade coating, aberration is impermissible for.In this case, surface of pigments is changed
The method of charge is preferable.This method eliminates color displacement, while it can also make larger change to viscosity.It has developed recently
A series of low viscosity di-iron trioxide, employs surface charge modifying method, and surface is made with inorganic charge modifying agent
Processing.This charge modifiers are the transition metal ions of low concentration, thus have no color displacement phenomenon, and viscosity can reduce
15KU or so.
The shortcomings that above method, when being handled with inorganic charge modifying agent iron oxide yellow surface, the mistake of additional low concentration
Metal ion is crossed, color displacement phenomenon is had no although being said on report, can so make the heavy metal ion of pigment exceeded, from
And other performances are more or less influenced, use occasion can be subject to certain restrictions.
The content of the invention
The present invention provides for deficiency of the prior art and is added without any metal ion or oxide, can quickly reduce
The method of di-iron trioxide viscosity.
In order to solve the above technical problems, the present invention adopts the following technical scheme that realization：
Technical grade di-iron trioxide filter cake material is predominantly carried out plus water mashing divides by the method for reducing di-iron trioxide viscosity
It dissipates, adjustment reaction solution pH value, high-speed stirred is filtered, rinsed afterwards for a period of time, and drying crushes, it is characterised in that：Adjust reaction solution
The process of pH value is：By technical grade di-iron trioxide filter cake material carry out plus water mashing it is scattered after add in reaction container and form concentration and be
10~14% slurries control 70~85 DEG C of temperature, and it is 9.0~9.5 then to add in lye and control material liquid PH value, high-speed stirred
3.5~4 it is small when.
Further, lye used in the adjustment reaction solution pH value is the Ionic Membrane of industrial 32% concentration --- it is pre-
10% concentration or so is diluted to, the high-speed stirred rotating speed is 350~400 revs/min.
Beneficial effects of the present invention：The advantage of the invention is that directly industrial higher level's di-iron trioxide filter cake material can be carried out
Technical finesse, controls certain slurry concentration, and pH value, temperature, speed of agitator and mixing time can cause di-iron trioxide
Viscosity be substantially reduced, so that the industrial common di-iron trioxide directly produced is being added without other metal ions and is helping
On the premise of agent, after above-mentioned relatively simple method, product viscosity has one to be substantially reduced, and has widened product significantly
Application field.
Specific embodiment
It elaborates with reference to specific embodiment to the present invention.
Embodiment 1
Be in 10 liters of stainless steel reaction bucket in volume, be previously added about 3 liters of tap water, then open strong stirring instrument into
Then 600 grams (meters of giving money as a gift) industrial 313 filter cake material of di-iron trioxide directly produced is added portionwise, makes its shape by row stirring
Into slurry, continue plus water management slurry concentration is 12% or so, and feed liquid is warming up to 70~75 degree and is kept, then slowly drip
Add the dilute alkali liquid of 10% concentration, PH is between 9.0~9.5 for control, and for control speed of agitator at 350~400 revs/min, stirring 1 is small
When after start to take out a small amount of sample (about 10 grams) and carry out analysis test, then proceed to stir, be sampled later when 1 is small.
The sample of taking-up, after suction filtration rinsing is up to standard, after worry cake is positioned over 110 DEG C of drying in oven, recycling micropulverizer crushes
Analysis test.Attached viscosity number test result is compared as follows shown in table：
Table 1:Viscosity number test result
| Temperature | PH value | Speed of agitator (rpm/min) | Mixing time (h) | Viscosity (KU) |
| 70~75 | 9.0~9.5 | 380 | 0.5h | 119.5 |
| 70~75 | 9.0~9.5 | 380 | 1.0h | 117.3 |
| 70~75 | 9.0~9.5 | 380 | 1.5h | 113.7 |
| 70~75 | 9.0~9.5 | 380 | 2.0h | 106.4 |
| 70~75 | 9.0~9.5 | 380 | 2.5h | 94.8 |
| 70~75 | 9.0~9.5 | 380 | 3.0h | 88.8 |
| 70~75 | 9.0~9.5 | 380 | 3.5h | 87.7 |
| 70~75 | 9.0~9.5 | 380 | 4.0h | 86.8 |
| 70~75 | 9.0~9.5 | 380 | 4.5h | 86.3 |
| 70~75 | 9.0~9.5 | 380 | 5.0h | 86.1 |
Remarks：The di-iron trioxide 313# filter cake material industrially produced directly dry, crush after, viscosity number test result
For：121.6KU.
It can be could see by table 1：Control slurry concentration 12% or so, 70~75 DEG C of temperature, PH=9.0~9.5, control are stirred
Mix rotating speed：380 revs/min, stirring 3.5 it is small when after, di-iron trioxide viscosity can be made to reduce 33.8KU, fall reaches
27.8%；Such as deferred reaction time again, though to be declined slightly the range of decrease substantially slow for viscosity number.So actual stirring 3.5~4 is small
When can be so that the viscosity of di-iron trioxide be substantially reduced.
Embodiment 2
In the case where 1 other conditions of example are constant, control the different pH value of reaction solution respectively, when stirring 3.5 is small after take
Go out sample and carry out analysis test.PH value is to the influence result such as following table of iron oxide yellow pigments yellow hue (yellow value degree) and viscosity：
Table 2：
For standard sample after directly being dried, crushed with the di-iron trioxide 313# filter cake material of before processing, detection color coloured light is：
| PH value | Mixing time | Yellow value degree (Δ b) | Viscosity (KU) |
| 7.0~7.5 | 3.5h | 0.12 | 120.2 |
| 7.5~8.0 | 3.5h | 0.17 | 118.6 |
| 8.0~8.5 | 3.5h | 0.23 | 105.1 |
| 8.5~9.0 | 3.5h | 0.18 | 94.8 |
| 9.0~9.5 | 3.5h | 0.11 | 87.7 |
| 9.5~10.0 | 3.5h | -0.32 | 85.8 |
| 10.0~10.5 | 3.5h | -0.76 | 84.7 |
| 10.5~11.0 | 3.5h | -1.28 | 84.2 |
| 11.0~11.5 | 3.5h | -1.79 | 83.9 |
It can be could see by table 2：In the case where other conditions are constant, with being continuously increased for reaction system PH, iron oxide yellow
The viscosity number of 313# gradually reduces, and in PH=9.0~9.5, the range of decrease is most apparent；When pH value be more than 9.5, as pH value constantly increases
Add, the viscosity number range of decrease of di-iron trioxide is slower and slower.
In addition, under the premise of other conditions are fixed, when between PH=7.0~9.5, the color of di-iron trioxide with it is former
Sample compares-- yellow hue (Δ b values) slightly rising, i.e., yellow phase degree is increased slightly；And work as pH value and be more than 9.5, yellow hue (Δ b
Value) become increasingly to bear instead, i.e., color can be graying.Thus, comprehensive iron oxide yellow viscosity considers together with colour index value, is ensureing
On the premise of iron oxide yellow colour index is unaffected, optimal PH=9.0~9.5 of above-mentioned reaction.
Above-described embodiment is merely illustrative of the technical solution of the present invention rather than the design of the present invention and protection domain is carried out
It limits, those of ordinary skill of the invention is modified or replaced equivalently technical scheme, without departing from technology
The objective and scope of scheme, should all cover in scope of the presently claimed invention.
Claims (3)
1. reducing the method for di-iron trioxide viscosity, predominantly technical grade di-iron trioxide filter cake material is carried out plus water mashing divides
It dissipates, adjustment reaction solution pH value, high-speed stirred is filtered, rinsed afterwards for a period of time, and drying crushes, it is characterised in that：Adjust reaction solution
The process of pH value is：By technical grade di-iron trioxide filter cake material carry out plus water mashing it is scattered after add in reaction container and form concentration and be
10~14% slurries control 70~85 DEG C of temperature, and it is 9.0~9.5 then to add in lye and control material liquid PH value, high-speed stirred
3.5~4 it is small when.
2. the method according to claim 1 for reducing di-iron trioxide viscosity, it is characterised in that：The adjustment reaction solution PH
Lye used in value is Ionic Membrane --- the pre-dilution to 10% concentration of industrial 32% concentration.
3. the method according to claim 1 for reducing di-iron trioxide viscosity, it is characterised in that：The high-speed stirred rotating speed
For 350~400 revs/min.
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| CN112111180A (en) * | 2020-08-18 | 2020-12-22 | 江苏宇星工贸有限公司 | Production process of low-viscosity iron oxide yellow |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112111180A (en) * | 2020-08-18 | 2020-12-22 | 江苏宇星工贸有限公司 | Production process of low-viscosity iron oxide yellow |
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Application publication date: 20180518 |