CN102618091A - Method for preparing free-flowing granular iron oxide yellow pigment - Google Patents
Method for preparing free-flowing granular iron oxide yellow pigment Download PDFInfo
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- CN102618091A CN102618091A CN2012100647402A CN201210064740A CN102618091A CN 102618091 A CN102618091 A CN 102618091A CN 2012100647402 A CN2012100647402 A CN 2012100647402A CN 201210064740 A CN201210064740 A CN 201210064740A CN 102618091 A CN102618091 A CN 102618091A
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Abstract
The invention discloses a method for preparing a free-flowing granular iron oxide yellow pigment. The method comprises the following steps of: preparing iron oxide yellow liquid slurry; and performing spray drying on the prepared iron oxide yellow liquid slurry on a spray tower for granulating. The granular iron oxide yellow pigment prepared through spray granulation by using the method has the characteristics of high spherical degree, uniform particles, particle diameter of 80-120 mum, and the like, so that the granular pigment has high free-flowing characteristic, convenience is brought to pipeline transmission of materials, automatic metering and the like in a use process, and the phenomenon of powder wall stagnation in pipelines and containers is avoided.
Description
Technical field
The present invention relates to a kind of method of manufacture of free flowing powder shape pigment, the ball shape ferric oxide yellow pigment particulate method of manufacture that particularly obtains through the liquid slurry spraying drying comprises two kinds or two above additives at least in this liquid slurry.
Background technology
Yellow oxide of iron claims that again iron carbonyl is called for short iron oxide yellow, is the more stable basic oxide of a kind of chemical property.Chemical molecular formula is Fe
2O
3H
2O or FeOOH are yellow meal.Color and luster has distinct pure ochre yellow, and has from lemon yellow to orange a series of coloured light.It is the aquo compound of aciculiform, has good pigment performance, and is all very high like tinting strength, opacifying power.
Ferric oxide yellow pigment is owing to there is good weathering resistance; Opacifying power and be used for process industry; The metope of building industry is whitewashed, and mosaic tile flooring and artificial marble and cement products painted also can be used as the tinting material of coating, You Mo ﹑ rubber and papermaking etc. simultaneously.Iron oxide yellow also can be used as the production iron oxide yellow in addition, and the catalyzer that raw material that iron oxide black and iron are green and chemical industry are used, the sugar-coat of pharmaceutically doing tablet Se ﹑ization Zhuan Pin ﹑ drawing etc.
Industry is at present gone up and is extensively adopted iron plate method explained hereafter yellow oxide of iron, and this technology has two steps usually: the first step is to prepare crystal seed in 20-50 centigradetemperatures with liquid caustic soda (or ammoniacal liquor) partly precipitated ferrous sulfate and bubbling air oxidation.With air, iron sheet and crystal seed make ferrous and airborne oxygen effect generate ferric iron and are deposited on the crystal seed in the ferrous sulfate medium then; Separate out sulfuric acid simultaneously; With iron sheet reacted ferrous sulfate, so constantly circulating reaction impels seed particles to grow up; Form hydrous iron oxide (being yellow oxide of iron) gradually, can obtain the ferric oxide yellow pigment of a series of form and aspect from light color to the dark color through control the coloured light progress.In recent years; Also have a kind of full liquid phase method technology also to can be used to produce iron oxide yellow, this technology crystal seed preparatory phase is identical with iron plate method technology, and different is in the oxidation reaction process in the presence of crystal seed; Drip ferrous sulfate and alkali (or ammonia) continuously; Make reaction system keep certain ferrous iron concentration and pH value, and, can obtain the ferric oxide yellow pigment of a series of form and aspect from light color to the dark color equally through control the coloured light progress without iron plate.Reaction finishes and removes impurity with sieve, and the water eccysis dissolubility salt that anhydrates carries out drying with drying room or banded moisture eliminator, pulverizes with kibbler then and obtains yellow oxide of iron powder pigment.
Present domestic ferric oxide yellow pigment final product form is Powdered; Because this pigment is in following process and use; Can produce a large amount of dust, be unfavorable for health of operators and environmental health, this powder-product is prone to produce wall sticking phenomenon in container and pipeline in addition; Can't carry out pipe-line transportation and reach automatic gauge accurately, thereby use occasion is restricted.
Though particulate iron oxide pigment method of manufacture was had report both at home and abroad: adopt the mechanical presses prilling process like German BAYER; Domestic Zhejiang Hangzhou Xiao Xiang pigment chemical industry ltd discloses a kind of particulate iron oxide yellow pigment and method of manufacture thereof, the patent No.: 03103924; Shanghai Yipin International Pigments Co., Ltd. discloses a kind of prilling process of powder pigment, the patent No.: 03115597; The two on croci pigment, sprays the certain quantity of fluid tackiness agent all through tablets press; Make powder pigment and tackiness agent under the high-speed stirring effect in bed around radially doing the high speed cyclotron motion; Bonded dose of powder surface of pigments is moistening, and particle runs foul of each other bonding, and particle diameter increases to processing requirement gradually; Adopt conventional method to carry out drying and screening then, obtain required granular pigments.
Above granulation all has following shortcoming, and the one, pigment has repetition exsiccant process, and product energy consumption is increased greatly; The 2nd, granules of pigments out-of-shape, sphericity are poor, not of uniform size, cause this particle free-flowing property poor, finally can influence use properties.
Summary of the invention
The objective of the invention is in order to overcome the two big shortcomings that above-mentioned mechanical pelleting exists, provide a kind of can unrestricted flow, do not have and glue that wall, particle physical strength are moderate, the particulate iron oxide yellow pigment of excellent dispersion.The one, can solve occupational illness problem, protection worker health that pigment industry dust pollution causes, improve Working environment; The 2nd, improve pigment and use industry mechanize, automatization level, raising work is renderd a service.
The present invention is achieved in that
(1) preparation iron oxide yellow liquid slurry
The yellow oxide of iron filter cake material (through sieving, wash, squeezing) that directly adopts our company to produce is earlier through slurry agitation vat (1300 millimeters of agitation vat diameter phi, high 1500 millimeters; The stirring blade diameter phi is 900 millimeters, mixing speed 0-80 rev/min, power of motor 15KW) carry out pre-dispersed to it; The batching of agitation vat is that standard is not (as in this scope with 40-50% iron oxide yellow solid content; Available a small amount of dry powder iron oxide yellow or tap water are regulated); And add additive in the dried weight 0.5 ~ 3.5% of iron oxide yellow, churning time: 30-45 minute, can obtain preliminary finely dispersed iron oxide yellow slurry.Then above-mentioned pre-dispersed iron oxide yellow slurry is passed through colloidal mill (output 3-10 ton again; Rotating speed 1600-5000 rev/min; Power of motor 37KW) circulation 15-30 minute, further to obtain particle fineness less than the iron oxide yellow slurry of 50 μ m (, returning mill) greater than the colloidal mill that returns of 50 μ m through 50 μ m screen clothes.
(2) utilize the above-mentioned iron oxide yellow liquid slurry for preparing on specific spray tower, to carry out spray drying granulation.The ultimate principle of spray granulating and drying machine is the slurry that has tackiness agent, sprays in the prilling tower with atomizer to atomize, and the droplet in the tower is dried to the particulate state powder by hot gas flow in the tower, draws off from the drying tower bottom then.
(3) spray tower and drying process parameter: spray tower diameter of phi=3000mm, high H=6300mm, spray tower heat-supplying mode is a gas furnace, the interior inlet air temperature of tower is that 350-380 ℃, exhaust temperature are 110-130 ℃, 70 ~ 110 kilograms/hour of feed pump flows.
(4) spraying gun form: centrifugal, spraying gun dispersion impeller diameter is 5000 ~ 15000 rev/mins of Φ=5.5mm, spraying gun rotating speeds; Pressure type, atomizer nozzle diameter are Φ=0.8mm, fresh feed pump pressure 2.2 ~ 3.0MP.
(5) particulate iron oxide that is obtained by above-mentioned centrifugal atomizer spray tower is yellow, through particle tested be sphere, particle diameter at 80 ~ 120 μ m, product moisture is 0.8 ~ 1.6%, tap density is 0.82 ~ 0.90 g/cm3; Particulate iron oxide by above-mentioned pressure atomizer spray tower obtains is yellow, and at 90 ~ 140 μ m, product moisture is 0.8 ~ 2.0% through particle tested type of being spherical (approximate apple shape), particle diameter, and tap density is 0.86 ~ 0.92g/cm3.Through analytical test: centrifugal still pressure atomizer spray tower obtains iron oxide yellow particulate free-flowing property, granule strength, dispersiveness and all meets the requirements.
(6), pelletizing additives is two kinds or two or more mixtures in calcium lignin sulphonate, aqurous ployurethane, vinyl resin sodium salt solution, ZX-I salt brine solution, methyl naphthalene sulfonic acid salt, water glass, sodium sulfate, the magnetic soil.
Advantage of the present invention is:
(1) the particulate iron oxide yellow pigment that obtains through present method mist projection granulating has good sphericity, uniform particles, particle diameter in characteristics such as 80 ~ 120 μ m; Thereby make the free-flowing character that this granular pigments is good; In use; Be convenient to material pipe conveying, automatic gauge etc., no powder wall stagnation behavior in pipeline and container.
(2) pelletizing additives that uses of the present invention can make in the pigment rapid drying process bonding fast, and pellet hardness is moderate, guarantees in transportation, to be rocked, slightly extruding and when in pipeline, adopting high-pressure delivery, also can not produce the grain breakage phenomenon.Can guarantee in use simultaneously that granules of pigments is prone to disperse in aqueous medium, use a small amount of mechanical external force, the short period of time can be uniformly dispersed.
(3) pelletizing additives according to the invention is a calcium lignin sulphonate, in this technology, plays (disperseing bonding) effect; Vinyl resin sodium salt solution, ZX-I salt brine solution play (disperseing bonding) effect in this technology; Water glass plays (bonding fast) effect in this technology; Sodium sulfate plays (dispersion) effect in this technology; Aqurous ployurethane plays (disperseing bonding fast) effect in this technology; Magnetic soil plays (bonding fast) effect in this technology.Traditional sticker such as gelatin etc. can not make material bonding fast or cohesive strength is too high causes dispersing property to make a difference, and part dispersion agent such as vinyl resin are answered the properties influence of material simultaneously, lose dispersion effect or poor effect.
Embodiment
Embodiment 1
(1), satisfactory yellow oxide of iron filter cake material is first with slurry agitation vat (1300 millimeters of agitation vat diameter phi, high 1500 millimeters; The stirring blade diameter phi is 900 millimeters, 80 rev/mins of mixing speed, power of motor 15KW) carry out pre-dispersedly, in above-mentioned slurry agitation vat, add 80 kilograms of tap water earlier; Then open and stir, add 12 kilograms of calcium lignin sulphonates and 4 kilograms of sodium sulfate according to this, continued stir about 5 minutes; Add the dried iron oxide yellow filter cake of counting 800 kilograms then pulls an oar in batches; Feeding intake finishes, and stirs shutdown in 40 minutes, the iron oxide yellow solid content that sampling records this moment 42% (like solid content not in the 40-50% scope; Available a small amount of dry powder iron oxide yellow or tap water are regulated, and the continuation stir about got final product in 15 minutes).Then above-mentioned pre-dispersed iron oxide yellow slurry was circulated 20 minutes through colloidal mill (3 ~ 10 tons/hour of output, 3100 rev/mins of rotating speeds, power of motor 37KW) again; So that obtain particle fineness less than the iron oxide yellow slurry of 50 μ m (, returning mill) greater than the colloidal mill that returns of 50 μ m through 50 μ m screen clothes.
(2), utilize the above-mentioned iron oxide yellow slurry for preparing to spray below and carry out spray drying granulation on the tower; This spray tower parameter is following: spray tower diameter of phi=3000mm; High H=6300mm, the spraying gun employing is centrifugal, the dispersion impeller diameter is Φ=5.5mm, and the inner heat-supplying mode of spray tower is a gas furnace.
(3), drying process parameter: spray tower inlet air temperature is 360-380 ℃, and exhaust temperature is 110-130 ℃, 7500 rev/mins of spraying gun rotating speeds, 90 kilograms/hour of feed pump flows.
(4), the particulate iron oxide that obtains through above-mentioned centrifugal atomizer spray tower is yellow, through the test color (with Powdered like product relatively) and other physical index as shown in table 1:
Table 1
Embodiment 2
(1), iron oxide yellow pulp preparation, spray tower parameter and drying process parameter are with embodiment 1.
(2), different with embodiment 1 be: spraying gun adopts pressure type, the atomizer nozzle diameter be Φ=0.8mm, fresh feed pump pressure-controlling at 2.5 ~ 2.7MP, 100 kilograms/hour of feed liquid flows.
(3), the particulate iron oxide that obtained by above-mentioned pressure atomizer spray tower is yellow, through the test color (with Powdered like product relatively) and other physical index as shown in table 2:
Table 2
Can find out from table 1, table 2: no matter be centrifugal or the yellow 313G of particulate iron oxide that obtains of pressure atomizer spray tower, its color and physical index are approximate; And both and Powdered like product 313 compare, and its tinctorial strength, color form and aspect basically become (total color difference △ E=0.38), meet color acceptability of color matches scope dictates (△ E≤1.0).Simultaneously; Particulate iron oxide is yellow relatively to have the high characteristics of tap density (tap density can improve about 30%) with Powdered like product; Thereby make the shared storage and the transportation stacking space of ferric oxide yellow pigment of equivalent weight reduce greatly, reduced storage and transportation cost.
Embodiment 3-7 method of manufacture are with embodiment 1, and additive dosage and spray tower main technical data are seen table 3 in the iron oxide yellow liquid slurry:
Table 3
The yellow product of the particulate iron oxide that embodiment 3-7 makes all can be obtained the 1 essentially identical effect with embodiment.
Claims (7)
1. the method for manufacture of a free flowing powder shape ferric oxide yellow pigment is characterized in that:
(1) preparation iron oxide yellow liquid slurry: after the pre-dispersed processing of yellow oxide of iron filter cake material process; Join slurries with 40-50% iron oxide yellow solid content; And adding is in the pelletizing additives of the dried weight 0.5 ~ 3.0% of iron oxide yellow; Churning time: 30-45 minute, obtain preliminary finely dispersed iron oxide yellow slurry, then above-mentioned pre-dispersed iron oxide yellow slurry is obtained the iron oxide yellow slurry of particle fineness less than 50 μ m through colloidal mill again;
(2) utilize the above-mentioned iron oxide yellow liquid slurry for preparing to carry out spray drying granulation on the tower in spray: the iron oxide black liquid slurry for preparing is sprayed in the prilling tower by 80 ~ 140 kilograms/hour flow and atomizes; And in tower, blast temperature and be 350-400 ℃ hot gas flow; Droplet in the tower is accomplished during freely falling body dry in tower; Be dried to the particulate state powder by hot gas flow in the tower, draw off from the drying tower bottom then.
2. the method for manufacture of a kind of free flowing powder shape ferric oxide yellow pigment according to claim 1; It is characterized in that: said spray tower diameter of phi=3000mm, high H=6300mm; Spray tower heat-supplying mode is a top spray hot gas; Inlet air temperature is that 350-380 ℃, exhaust temperature are 110-130 ℃ in the tower, 70 ~ 110 kilograms/hour of feed pump flows; Spraying gun is established in the bottom of said spray tower.
3. the method for manufacture of a kind of free flowing powder shape ferric oxide yellow pigment according to claim 1 is characterized in that: said mist projection granulating spraying gun form can be chosen centrifugal or pressure type wantonly.
4. the method for manufacture of a kind of free flowing powder shape ferric oxide yellow pigment according to claim 3 is characterized in that: said centrifugal atomizer dispersion impeller diameter is 5000 ~ 15000 rev/mins of Φ=5.5mm, spraying gun rotating speeds.
5. the method for manufacture of a kind of free flowing powder shape ferric oxide yellow pigment according to claim 3 is characterized in that: said pressure atomizer nozzle diameter is Φ=0.8mm, fresh feed pump pressure 2.2 ~ 3.0MP.
6. the method for manufacture of a kind of free flowing powder shape ferric oxide yellow pigment according to claim 1 is characterized in that: pelletizing additives is two kinds or two or more mixtures in calcium lignin sulphonate, aqurous ployurethane, vinyl resin sodium salt solution, ZX-I salt brine solution, methyl naphthalene sulfonic acid salt, water glass, sodium sulfate, the magnetic soil.
7. according to the method for manufacture of the described a kind of free flowing powder shape ferric oxide yellow pigment of claim 1, it is characterized in that: said pelletizing additives consumption is 0.5 ~ 3.5% of the dried meter of an iron oxide yellow weight.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105602291A (en) * | 2016-02-17 | 2016-05-25 | 升华集团德清华源颜料有限公司 | Method for improving hue of particle iron oxide yellow pigment |
| CN112646394A (en) * | 2021-01-12 | 2021-04-13 | 国泰新科工业科技(宜兴)有限公司 | Preparation method of hollow granular inorganic pigment |
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| CN1195006A (en) * | 1997-02-10 | 1998-10-07 | 拜尔公司 | Inorganic pigment pellets for coloring plastics, lacquers and building materials and process for production thereof |
| CN1923708A (en) * | 2006-09-22 | 2007-03-07 | 湖南三环颜料有限公司 | Producing method of iron oxide yellow pigment |
| CN101824235A (en) * | 2010-04-29 | 2010-09-08 | 南通宝聚颜料有限公司 | Preparation process of medium temperature resistant iron oxide yellow |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105602291A (en) * | 2016-02-17 | 2016-05-25 | 升华集团德清华源颜料有限公司 | Method for improving hue of particle iron oxide yellow pigment |
| CN112646394A (en) * | 2021-01-12 | 2021-04-13 | 国泰新科工业科技(宜兴)有限公司 | Preparation method of hollow granular inorganic pigment |
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Application publication date: 20120801 |