CN112111179B - Production process of heat-resistant iron oxide black - Google Patents

Production process of heat-resistant iron oxide black Download PDF

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CN112111179B
CN112111179B CN202010830902.3A CN202010830902A CN112111179B CN 112111179 B CN112111179 B CN 112111179B CN 202010830902 A CN202010830902 A CN 202010830902A CN 112111179 B CN112111179 B CN 112111179B
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iron oxide
oxide black
surfactant
coupling agent
refractory material
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CN112111179A (en
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单淼
陆云飞
宋润亮
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Jiangsu Yuxing Technology Co ltd
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Jiangsu Yuxing Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/22Compounds of iron
    • C09C1/24Oxides of iron
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/08Ferroso-ferric oxide [Fe3O4]
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    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/003Flushing
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041Grinding
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/043Drying, calcination
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    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08Treatment with low-molecular-weight non-polymer organic compounds
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT 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
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12Treatment with organosilicon compounds

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a production process of heat-resistant iron oxide black, which belongs to the field of chemical pigments and can be used for preparing an iron oxide black filter cake by a sodium hydroxide oxidation method, dehydrating and drying the iron oxide black filter cake, preliminarily preparing powder, mixing the powder with white carbon black and a powdery refractory material, dispersing the mixture at a high speed uniformly, innovatively introducing a carrying device, and carrying a surfactant and a coupling agent by absolute ethyl alcohol steam in a clamping manner based on the fluidity and the contact property of gas to promote the powdery refractory material to uniformly and comprehensively cover the surface of the iron oxide black, so that a layer of compact high-temperature-resistant film is not easily formed, the temperature resistance of the iron oxide black is remarkably improved, and meanwhile, the acid resistance, the alkali resistance, the light absorption property, the tinting strength, the compatibility and the dispersibility are greatly improved.

Description

Production process of heat-resistant iron oxide black
Technical Field
The invention relates to the field of chemical pigments, in particular to a production process of heat-resistant iron oxide black.
Background
Iron-based pigments are important inorganic color pigments, and their annual output is the first of inorganic color pigments. Due to the enhancement of the environmental protection consciousness of the world, the inorganic iron series pigment continuously replaces organic pigments and lead series and chromium series toxic inorganic pigments such as red lead, lead chrome yellow and the like by the characteristics of no toxicity, no odor, no pollution and the like. The iron oxide black has simple chemical components, no toxicity, no pollution and strong chemical stability, and is widely applied to paint coatings in the building industry.
However, iron oxide black is dehydrated and oxidized into iron oxide red when the temperature reaches about 100 ℃, and the iron oxide black is discolored and discolored when used in some occasions with higher temperature, so that the application range of the iron oxide black is limited.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a production process of heat-resistant iron oxide black, which can be used for preparing an iron oxide black filter cake by a sodium hydroxide oxidation method, then dehydrating and drying the iron oxide black filter cake, preliminarily preparing powder, mixing the powder with white carbon black and a powdery refractory material, dispersing the powder uniformly at a high speed, innovatively introducing a clamping and carrying device, and promoting the powdery refractory material to uniformly and comprehensively cover the surface of the iron oxide black by using anhydrous ethanol steam in a mode of clamping and carrying a surfactant and a coupling agent based on the fluidity and the contact property of gas, so that a compact high-temperature-resistant film is formed, the temperature resistance of the iron oxide black is obviously improved, and the acid resistance, the alkali resistance, the light absorption property, the tinting strength, the compatibility and the dispersibility are greatly improved.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A production process of heat-resistant iron oxide black comprises the following steps:
s1, filtering the solution prepared by the sodium hydroxide oxidation method of the raw materials, and then filtering the solution in a filter press to obtain a solid which is an iron oxide black filter cake;
s2, dehydrating and drying the iron oxide black filter cake at 80-150 ℃, and crushing the dried iron oxide black pigment to obtain primary powder of 50-80 meshes;
s3, mixing white carbon black accounting for 5-8% of the weight of the primary powder with the powdery refractory material, and dispersing at a high speed of 1500-2000rpm for 15-20 min;
s4, taking excessive absolute ethyl alcohol, heating to 80 ℃ to obtain ethyl alcohol steam, and mixing with the surfactant and the coupling agent in turn in the carrying device;
s5, guiding the mixed steam to the mixed powder for covering and impacting, standing and cooling for 1-2 hours after the consumption of the auxiliary agent is finished;
s6, taking out, washing with absolute ethyl alcohol for 2-3 times, vacuum drying at 50-60 ℃ for 4-5h, grinding, and sieving with a 60-mesh sieve to obtain the finished product of the heat-resistant iron oxide black.
Furthermore, the adding ratio of the white carbon black to the powdery refractory material is 1:1-5, and the particle size of the powdery refractory material is kept between 10 and 50 mu m.
Further, the refractory material includes, but is not limited to, alumina, lanthana, beryllia, calcium oxide, zirconia, uranium oxide, magnesium oxide, cerium oxide, thoria, silicon carbide, titanium carbide, tantalum carbide, boron nitride, silicon nitride, zirconium boride, titanium boride, hafnium boride, and molybdenum disilicide.
Further, the surfactant is one of rosin amine and abietic acid, and the dosage of the surfactant is 0.2-0.4% of the primary powder.
Furthermore, the coupling agent adopts one of vinyltriethoxysilane, trimethylethoxysilane and diphenyldiethoxysilane, and the dosage of the coupling agent accounts for 0.1-0.2% of the original powder.
Further, the surfactant and the coupling agent in step S4 should be preheated to 80-100 ℃ before mixing with the ethanol vapor.
Further, the clamp is taken the device and is held the liquid ball including holding, it installs electric heating ball in the liquid ball to hold, it is connected with the clamp and takes the pipe to hold the liquid ball upper end, the clamp is taken the pipe and is gone up the symmetry and install a pair of spherical shower nozzle, the clamp is taken a tub rear end downside and is connected with the cladding fill that is linked together, the cladding is fought the lower extreme and is connected with the recovery tube, the cladding is fought the in-connection and is connected with the clad plate, set up a plurality of evenly distributed's ventilative micropore on the clad plate, through the characteristics of the spherical shower nozzle of symmetry installation, utilize surfactant agent and coupling agent under mutual convection current impact, disperse into more small liquid pearl, help being pressed from both sides by ethanol steam and taking, the preliminary mixing of while convection current impact in-process also, more direct and abundant when the cladding is fought and iron oxide black raw materials contact.
Further, the cladding plate lower extreme is connected with a plurality of evenly distributed's elasticity fulcrum ball, and crisscross distribution between elasticity fulcrum ball and the ventilative micropore, elasticity fulcrum ball both ends are connected with the biography power piece of symmetric distribution, biography power piece upper end is connected with the turn-over stick, and in the turn-over stick extended to ventilative micropore, based on the instability of air current, can force the turn-over stick to form high frequency vibrations in respective ventilative micropore, forces the iron oxide black raw materials of top to ceaselessly roll, improves its and ethanol steam's contact degree to improve the cladding effect.
Further, the turn-over stick includes top ball and connects the extension stick that pushes up the ball lower extreme on, and extends the stick and connect in the biography power piece upper end, it has the cotton layer of imbibition to go up the parcel of top ball outer end, and the cotton layer of imbibition not only can adsorb ethanol steam and then releases when receiving the extrusion in ventilative micropore, not only can guarantee the sufficiency of ethanol in the cladding process to can dissolve surfactant active and coupling agent and play the cladding effect, its expanded characteristic can promote the black raw materials of iron oxide to improve the effect of rolling simultaneously.
Further, the air-permeable micropores are smaller than the particle size of the primary powder, and the ratio of the shortest distance between adjacent air-permeable micropores to the particle size of the primary powder is 0.9-0.95: 1, the impact effect of the airflow on the turnover rod can be improved, the iron oxide black raw material can be enabled to change positions through rolling between the ventilation micropores, the coating dead angle is not easy to occur, and the iron oxide black raw material can be comprehensively contacted with ethanol steam.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) this scheme can realize adopting the sodium hydroxide oxidation legal system to prepare dehydration stoving behind the iron oxide black filter cake, and preliminary powder process mixes with white carbon and powdered refractory material, after high-speed homodisperse again, innovative introduction presss from both sides and carries the device, utilize absolute ethyl alcohol steam to press from both sides and carry surfactant active, the mode of coupling agent, based on the mobility and the contact nature of gas, impel powdered refractory material at the even and comprehensive cover in iron oxide black surface, the cladding dead angle is difficult for appearing, form the high temperature resistant film that the one deck is fine and close, show the temperature resistance who improves iron oxide black, simultaneously acidproof, alkali-resisting and light absorption, the tinting strength, compatibility, the dispersibility all obtains promoting by a wide margin.
(2) The clamp is taken the device and is including holding the liquid ball, it installs electric heating ball in the liquid ball to hold, it is connected with the clamp and takes the pipe to hold the liquid ball upper end, the clamp is taken the symmetry on the pipe and is installed a pair of spherical shower nozzle, the clamp is taken a tub tail end downside and is connected with the cladding fill that is linked together, the cladding is fought the lower extreme and is connected with the recovery tube, the cladding is fought the in-connection and is connected with the cladding plate, set up a plurality of evenly distributed's ventilative micropore on the cladding plate, characteristics through the spherical shower nozzle of symmetry installation, utilize surfactant and coupling agent under mutual convection current strikes, disperse into more small liquid pearl, help being carried by ethanol steam clamp, the convection current strikes the in-process simultaneously and also can tentatively mix, it is more direct and abundant when fighting with the black raw materials of iron oxide in the cladding.
(3) Cladding plate lower extreme is connected with a plurality of evenly distributed's elasticity fulcrum ball, and crisscross distribution between elasticity fulcrum ball and the ventilative micropore, elasticity fulcrum ball both ends are connected with the biography power piece of symmetric distribution, it is connected with the turn-over stick to pass power piece upper end, and the turn-over stick extends to in the ventilative micropore, instability based on the air current, can force the turn-over stick to form high frequency vibrations in respective ventilative micropore, the black raw materials of iron oxide who forces the top dynamic that does not stop rolls, improve its and ethanol steam's degree of contact, thereby improve the cladding effect.
(4) The turn-over stick includes top ball and connects the extension stick of top ball lower extreme on, and extends the stick and connect in the biography power piece upper end, and it has the cotton layer of imbibition to go up top ball outer end parcel, and the cotton layer of imbibition not only can adsorb ethanol steam then releases when receiving the extrusion in ventilative micropore, not only can guarantee the sufficiency of ethanol in the cladding process to can dissolve surfactant active and coupling agent and come the performance cladding effect, its expanded characteristic can promote the black raw materials of iron oxide to improve the effect of rolling simultaneously.
(5) The air-permeable micropores are smaller than the particle size of the primary powder, and the ratio of the shortest distance between adjacent air-permeable micropores to the particle size of the primary powder is 0.9-0.95: 1, the impact effect of the airflow on the turnover rod can be improved, the iron oxide black raw material can be enabled to change positions through rolling between the ventilation micropores, the coating dead angle is not easy to occur, and the iron oxide black raw material can be comprehensively contacted with ethanol steam.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a schematic view of a clip carrying device according to the present invention;
FIG. 3 is a schematic view of the structure of the tube-carrying portion of the present invention;
FIG. 4 is a schematic view of the structure of the containment hopper of the present invention;
FIG. 5 is a schematic view of the structure at A in FIG. 4;
fig. 6 is a schematic structural view of the turn-over bar of the present invention.
The reference numbers in the figures illustrate:
1 liquid storage ball, 2 electric heating balls, 3 clamping and carrying pipes, 4 coating hoppers, 5 recovery pipes, 6 spherical nozzles, 7 coating plates, 8 elastic fulcrum balls, 9 turnover rods, 91 upper jacking balls, 92 extending rods, 93 liquid absorption cotton layers and 10 force transmission sheets.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by those skilled in the art without any inventive work are within the scope of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1-2, a process for producing a heat-resistant black iron oxide, includes the following steps:
s1, filtering the solution prepared by the sodium hydroxide oxidation method of the raw materials, and then filtering the solution in a filter press to obtain a solid which is an iron oxide black filter cake;
s2, dehydrating and drying the iron oxide black filter cake at 80 ℃, and crushing the dried iron oxide black pigment to obtain primary powder of 50-80 meshes;
s3, taking white carbon black accounting for 5 percent of the weight of the primary powder and a powdery refractory material to mix, and dispersing at a high speed of 1500rpm for 15 min;
s4, taking excessive absolute ethyl alcohol, heating to 80 ℃ to obtain ethyl alcohol steam, and mixing with the surfactant and the coupling agent in turn in the carrying device;
s5, guiding the mixed steam to the mixed powder for covering and impacting, and standing and cooling for 1h after the consumption of the auxiliary agent is finished;
s6, taking out, washing with absolute ethyl alcohol for 2 times, vacuum drying at 50 ℃ for 4h, grinding, and sieving with a 60-mesh sieve to obtain the finished product of the heat-resistant iron oxide black.
The adding ratio of the white carbon black to the powdery refractory material is 1:5, and the particle size of the powdery refractory material is kept between 10 and 50 mu m.
The refractory material is alumina.
The surfactant is abietic acid, and the dosage of the surfactant is 0.2% of the primary powder.
The coupling agent adopts vinyl triethoxysilane, and the dosage of the coupling agent accounts for 0.1% of the primary powder.
The surfactant and coupling agent in step S4 should be preheated to 80 ℃ before mixing with the ethanol vapor.
Please refer to fig. 2-3, the clamp-carrying device comprises a liquid storage ball 1, an electric heating ball 2 is installed in the liquid storage ball 1, the upper end of the liquid storage ball 1 is connected with a clamp-carrying pipe 3, a pair of spherical nozzles 6 are symmetrically installed on the clamp-carrying pipe 3, the lower side of the tail end of the clamp-carrying pipe 3 is connected with a coating bucket 4 which is communicated, the lower end of the coating bucket 4 is connected with a recovery pipe 5, the coating bucket 4 is connected with a coating plate 7, the coating plate 7 is provided with a plurality of uniformly distributed air-permeable micropores, the spherical nozzles 6 are symmetrically installed, the surfactant and the coupling agent are utilized to disperse into more tiny liquid beads under mutual convection impact, the liquid beads are favorably clamped and carried by ethanol steam, meanwhile, the convection impact process can be also primarily mixed, and the coating bucket 4 is more directly and fully contacted with iron oxide black raw materials.
Referring to fig. 4, the lower end of the cladding plate 7 is connected with a plurality of elastic fulcrum balls 8 which are uniformly distributed, the elastic fulcrum balls 8 and the air-permeable micropores are distributed in a staggered manner, two ends of each elastic fulcrum ball 8 are connected with force transmission pieces 10 which are symmetrically distributed, the upper ends of the force transmission pieces 10 are connected with turnover rods 9, and the turnover rods 9 extend into the air-permeable micropores, so that the turnover rods 9 can be forced to form high-frequency vibration in the respective air-permeable micropores based on the instability of air flow, the iron oxide black raw material above the turnover rods can be forced to continuously and dynamically roll, the contact degree of the iron oxide black raw material with ethanol steam is improved, and the cladding effect is improved.
Referring to fig. 5, the turn-over bar 9 includes an upper top ball 91 and an extension bar 93 connected to the lower end of the upper top ball 91, the extension bar 93 is connected to the upper end of the force-transmitting plate 10, the outer end of the upper top ball 91 is wrapped with a liquid-absorbing cotton layer 92, the liquid-absorbing cotton layer 92 can absorb ethanol vapor and then release the ethanol vapor when being extruded in the air-permeable micropores, and not only can the sufficient performance of ethanol in the wrapping process be ensured, so that the surfactant and the coupling agent can be dissolved to play a wrapping role, but also the expansion characteristic of the liquid-absorbing cotton layer 92 can push the iron oxide black raw material to improve the rolling effect.
The air-permeable micropores are smaller than the particle size of the primary powder, and the ratio of the shortest distance between adjacent air-permeable micropores to the particle size of the primary powder is 0.9-0.95: 1, the impact effect of the airflow on the turnover rod 9 can be improved, and the iron oxide black raw material can be enabled to change positions through rolling between the ventilation micropores, so that the iron oxide black raw material is not easy to wrap dead corners, and can be comprehensively contacted with ethanol steam.
Example 2:
referring to fig. 1-2, a process for producing a heat-resistant black iron oxide, includes the following steps:
s1, filtering the solution prepared by the sodium hydroxide oxidation method of the raw materials, and then filtering the solution in a filter press to obtain a solid which is an iron oxide black filter cake;
s2, dehydrating and drying the iron oxide black filter cake at 100 ℃, and crushing the dried iron oxide black pigment to obtain primary powder of 50-80 meshes;
s3, taking white carbon black with 6 percent of the weight of the primary powder and powdery refractory material to mix, and dispersing at a high speed of 1800rpm for 20 min;
s4, taking excessive absolute ethyl alcohol, heating to 80 ℃ to obtain ethyl alcohol steam, and mixing with the surfactant and the coupling agent in turn in the carrying device;
s5, guiding the mixed steam to the mixed powder for covering and impacting, standing and cooling for 1.5h after the consumption of the auxiliary agent is finished;
s6, taking out, washing with absolute ethyl alcohol for 2 times, vacuum drying at 55 ℃ for 4h, grinding, and sieving with a 60-mesh sieve to obtain the finished product of the heat-resistant iron oxide black.
The adding ratio of the white carbon black to the powdery refractory material is 1:3, and the particle size of the powdery refractory material is kept between 10 and 50 mu m.
The refractory material is alumina.
The surfactant is abietic acid, and the dosage of the surfactant is 0.3% of the primary powder.
The coupling agent adopts vinyl triethoxysilane, and the dosage of the coupling agent accounts for 0.15% of the primary powder.
The surfactant and coupling agent in step S4 should be preheated to 80-100 c before mixing with the ethanol vapor.
The remainder was in accordance with example 1.
Example 3:
referring to fig. 1-2, a process for producing a heat-resistant black iron oxide, includes the following steps:
s1, filtering the solution prepared by the sodium hydroxide oxidation method of the raw materials, and then filtering the solution in a filter press to obtain a solid which is an iron oxide black filter cake;
s2, dehydrating and drying the iron oxide black filter cake at 150 ℃, and crushing the dried iron oxide black pigment to obtain primary powder of 50-80 meshes;
s3, taking white carbon black accounting for 8 percent of the weight of the primary powder and a powdery refractory material to mix, and dispersing at a high speed of 2000rpm for 20 min;
s4, taking excessive absolute ethyl alcohol, heating to 80 ℃ to obtain ethyl alcohol steam, and mixing with the surfactant and the coupling agent in turn in the carrying device;
s5, guiding the mixed steam to the mixed powder for covering and impacting, and standing and cooling for 2 hours after the consumption of the auxiliary agent is finished;
s6, taking out, washing with absolute ethyl alcohol for 3 times, vacuum drying at 60 ℃ for 5h, grinding, and sieving with a 60-mesh sieve to obtain the finished product of the heat-resistant iron oxide black.
The adding ratio of the white carbon black to the powdery refractory material is 1:1, and the particle size of the powdery refractory material is kept between 10 and 50 mu m.
The refractory material is alumina.
The surfactant is abietic acid, and the dosage of the surfactant is 0.4% of the primary powder.
The coupling agent adopts vinyl triethoxysilane, and the dosage of the coupling agent accounts for 0.2% of the primary powder.
The surfactant and coupling agent in step S4 should be preheated to 100 ℃ before mixing with the ethanol vapor.
The remainder was in accordance with example 1.
The invention can realize that the iron oxide black filter cake is prepared by a sodium hydroxide oxidation method, then is dehydrated and dried, is preliminarily prepared into powder, is mixed with the white carbon black and the powdery refractory material, is dispersed uniformly at a high speed, is innovatively introduced into a carrying device, utilizes a mode of carrying a surfactant and a coupling agent by absolute ethyl alcohol steam, and promotes the powdery refractory material to uniformly and comprehensively cover the surface of the iron oxide black based on the fluidity and the contact property of gas, so that a coating dead angle is not easy to appear, a compact high-temperature-resistant film is formed, the temperature resistance of the iron oxide black is obviously improved, and meanwhile, the acid resistance, the alkali resistance, the light absorption property, the tinting strength, the compatibility and the dispersibility are greatly improved.
The above are merely preferred embodiments of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.

Claims (7)

1. A production process of heat-resistant iron oxide black is characterized by comprising the following steps: the method comprises the following steps:
s1, filtering the solution prepared by the sodium hydroxide oxidation method of the raw materials, and then filtering the solution in a filter press to obtain a solid which is an iron oxide black filter cake;
s2, dehydrating and drying the iron oxide black filter cake at 80-150 ℃, and crushing the dried iron oxide black pigment to obtain primary powder of 50-80 meshes;
s3, mixing white carbon black and powdery refractory material which are 5-8% of the weight of the primary powder with the primary powder, and dispersing at a high speed of 1500-2000rpm for 15-20 min;
s4, taking excessive absolute ethyl alcohol, heating to 80 ℃ to obtain ethyl alcohol vapor, and mixing with the surfactant and the coupling agent in turn in the carrying device;
s5, guiding the mixed steam to the mixed powder for covering and impacting, standing and cooling for 1-2 hours after the consumption of the auxiliary agent is finished;
s6, taking out, washing with absolute ethyl alcohol for 2-3 times, vacuum drying at 50-60 ℃ for 4-5h, grinding, and sieving with a 60-mesh sieve to obtain the finished product of heat-resistant iron oxide black;
the surfactant and the coupling agent in the step S4 are preheated to 80-100 ℃ before being mixed with the ethanol vapor;
the clamping and carrying device comprises a liquid storage ball (1), an electric heating ball (2) is mounted in the liquid storage ball (1), the upper end of the liquid storage ball (1) is connected with a clamping and carrying pipe (3), a pair of spherical spray heads (6) are symmetrically mounted on the clamping and carrying pipe (3), the lower side of the tail end of the clamping and carrying pipe (3) is connected with a communicated coating bucket (4), the lower end of the coating bucket (4) is connected with a recovery pipe (5), a coating plate (7) is connected in the coating bucket (4), and a plurality of uniformly distributed air-permeable micropores are formed in the coating plate (7); the surfactant and the coupling agent carried by the ethanol vapor are contacted with the iron oxide black in the coating hopper (4);
cladding plate (7) lower extreme is connected with a plurality of evenly distributed's elasticity fulcrum ball (8), and crisscross distribution between elasticity fulcrum ball (8) and the ventilative micropore, elasticity fulcrum ball (8) both ends are connected with the biography power piece (10) of symmetric distribution, pass power piece (10) upper end is connected with turn-over stick (9), and turns over in stick (9) extends to ventilative micropore.
2. The process for producing heat-resistant iron oxide black according to claim 1, wherein: the adding ratio of the white carbon black to the powdery refractory material is 1:1-5, and the particle size of the powdery refractory material is kept between 10 and 50 mu m.
3. The process for producing heat-resistant iron oxide black according to claim 2, wherein: the refractory material comprises aluminum oxide, lanthanum oxide, beryllium oxide, calcium oxide, zirconium oxide, uranium oxide, magnesium oxide, cerium oxide, thorium oxide, silicon carbide, titanium carbide, tantalum carbide, boron nitride, silicon nitride, zirconium boride, titanium boride, hafnium boride and molybdenum disilicide.
4. The process for producing heat-resistant iron oxide black according to claim 1, wherein: the surfactant is one of rosin amine and abietic acid, and the dosage of the surfactant is 0.2-0.4% of the primary powder.
5. The process for producing heat-resistant iron oxide black according to claim 1, wherein: the coupling agent adopts one of vinyl triethoxysilane, trimethylethoxysilane and diphenyldiethoxysilane, and the amount of the coupling agent is 0.1-0.2% of the primary powder.
6. The process for producing heat-resistant iron oxide black according to claim 1, wherein: turn-over stick (9) are including last kickball (91) and connect in extension stick (93) of last kickball (91) lower extreme, and extend stick (93) and connect in biography power piece (10) upper end, it has imbibition cotton layer (92) to go up kickball (91) outer end parcel.
7. The process for producing heat-resistant iron oxide black according to claim 1, wherein: the air-permeable micropores are smaller than the particle size of the primary powder, and the ratio of the shortest distance between every two adjacent air-permeable micropores to the particle size of the primary powder is 0.9-0.95: 1.
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CN103819940A (en) * 2014-02-12 2014-05-28 铜陵瑞莱科技有限公司 Fire-retardant black iron oxide pigment
CN106084895A (en) * 2016-06-02 2016-11-09 凤台精兴生物科技有限公司 A kind of Flame-retardant iron oxide black pigment and preparation method thereof
CN207659114U (en) * 2017-12-08 2018-07-27 安徽新涛新材料科技股份有限公司 A kind of secondary surface modifying apparatus of super fine calcium carbonate powder

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DK1991329T3 (en) * 2006-02-21 2013-01-07 Council Scient Ind Res Beam impeller atomizer for spray drying and method for producing finely dispersed slurry / liquid spray

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Publication number Priority date Publication date Assignee Title
CN103819940A (en) * 2014-02-12 2014-05-28 铜陵瑞莱科技有限公司 Fire-retardant black iron oxide pigment
CN106084895A (en) * 2016-06-02 2016-11-09 凤台精兴生物科技有限公司 A kind of Flame-retardant iron oxide black pigment and preparation method thereof
CN207659114U (en) * 2017-12-08 2018-07-27 安徽新涛新材料科技股份有限公司 A kind of secondary surface modifying apparatus of super fine calcium carbonate powder

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