CN112126252A - Production process of heat-resistant iron oxide yellow - Google Patents

Production process of heat-resistant iron oxide yellow Download PDF

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Publication number
CN112126252A
CN112126252A CN202010831630.9A CN202010831630A CN112126252A CN 112126252 A CN112126252 A CN 112126252A CN 202010831630 A CN202010831630 A CN 202010831630A CN 112126252 A CN112126252 A CN 112126252A
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iron oxide
oxide yellow
fixedly connected
mixing box
wall
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CN112126252B (en
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单淼
陆云飞
宋润亮
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Jiangsu Yuxing Industry And Trade Co ltd
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Jiangsu Yuxing Industry And Trade 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
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    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]
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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
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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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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    • 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
    • C09C3/063Coating
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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
    • C09C3/08Treatment 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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Abstract

The invention discloses a production process of heat-resistant iron oxide yellow, belonging to the technical field of iron oxide yellow production, and the production process of the heat-resistant iron oxide yellow comprises the following steps: s1, mixing the raw materials; s2, oxidizing; s3, impurity removal and subsequent treatment; s4, adding a coating agent; s5, processing materials; s6, neutralizing and aging; and S7, performing solid-liquid separation. The organic silicon modified resin is creatively selected and added in the preparation process of the ferrous oxide, has the characteristics of corrosion resistance, oxidation resistance and high temperature resistance, can adapt to the preparation environment of the iron oxide yellow, cannot be damaged, can effectively improve the heat resistance of the iron oxide yellow, can carry out surface coating on the prepared iron oxide yellow through reasonable design of the components and the mass ratio of the coating agent, design of a combined process method and arrangement of a material treatment device, further improves the heat resistance, and greatly improves the application range of the iron oxide yellow.

Description

Production process of heat-resistant iron oxide yellow
Technical Field
The invention relates to the technical field of iron oxide yellow production, and particularly relates to a production process of heat-resistant iron oxide yellow.
Background
The iron oxide pigment is an inorganic pigment with wide application, wherein the iron oxide yellow has bright color and luster, the chromatic light is between lemon yellow and orange yellow, and the iron oxide pigment has high pigment quality. The iron oxide yellow is not only a high-quality pigment, but also can be dehydrated and discolored to become iron oxide red under the conditions of 150 ℃ and 200 ℃, so that the iron oxide yellow can also be used as a raw material of the iron oxide red.
The air oxidation method is the most common production method of iron oxide yellow, and is mainly divided into two steps: 1. preparing ferric oxide seed crystal, namely reacting ferrous sulfate with sodium hydroxide to prepare ferrous hydroxide; 2. pumping the prepared ferric oxide seed crystal into an oxidation barrel, mixing with iron and sulfuric acid, introducing steam for heating, controlling the temperature of the mixture at the reaction temperature, introducing air into the reaction system, oxidizing ferrous sulfate by using oxygen in the air to generate Fe2O3·H2And growing gradually by taking the seed crystal as a core until the color of the seed crystal meets the requirements of the standard sample.
The iron oxide yellow prepared in the prior art has poor heat resistance, can be dehydrated and discolored under the conditions of 150 ℃ plus 200 ℃, and can be changed into iron oxide red through deterioration, so that the iron oxide yellow pigment cannot be applied to high-temperature occasions such as plastic processing, baking type coatings and the like, and the application range of the iron oxide yellow is greatly 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 yellow, which can be used for creatively selecting and adding organic silicon modified resin in the preparation process of ferrous oxide, wherein the organic silicon modified resin has the characteristics of corrosion resistance, oxidation resistance and high temperature resistance, can adapt to the preparation environment of the iron oxide yellow, cannot be damaged, and can effectively improve the heat resistance of the iron oxide yellow.
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 yellow comprises the following steps:
s1, mixing the raw materials: adding a proper amount of calcium carbonate, organic silicon modified resin and water into a reaction kettle, introducing air and stirring, and then adding a corresponding amount of ferrous chloride into the reaction kettle;
s2, oxidation: adjusting the temperature of the reaction kettle to 85-90 ℃, continuously blowing air into the reaction kettle in the process until the required color is obtained, preserving the heat for 45-65min, and discharging;
s3, impurity removal and subsequent treatment: after discharging, adding a dilute hydrochloric acid solution to remove redundant calcium carbonate, and then rinsing, filter pressing, drying and crushing to obtain iron oxide yellow containing the organic silicon modified resin;
s4, adding a coating agent: weighing a proper amount of coating agent, putting the coating agent into a ball milling cylinder of a material processing device, weighing the iron oxide yellow prepared in the corresponding amount S3, and putting the iron oxide yellow into the ball milling cylinder in the same way;
s5, material processing: injecting a proper amount of clear water into the mixing box through a water inlet pipe, starting a driving motor to drive a ball milling cylinder to rotate, carrying out ball milling and stirring mixing treatment on a coating agent and iron oxide yellow, obtaining a preliminary mixture after 2 hours, closing a motor base, opening a valve on a material guide pipe, guiding the preliminary mixture into a dispersion box, carrying out ultrasonic dispersion treatment on the preliminary mixture, treating for 3 hours to obtain a final mixture, and discharging the final mixture through a material discharge pipe;
s6, neutralizing and aging: slowly dropwise adding ethyl acetate into the final mixture in the S5 while stirring until the pH value of the mixed solution is neutral, and then standing and aging;
s7, solid-liquid separation: and (4) centrifugally separating the aged mixed solution in the S6, wet-grinding the solid material by using a three-roll grinder, and drying to obtain the iron oxide yellow with the surface coated with the oil-containing organic silicon modified resin.
Further, the material processing device in the S4 comprises a mixing box and a dispersing box arranged below the mixing box, wherein two symmetrically arranged support rods are fixedly connected to the top end of the dispersing box, the top ends of the support rods are fixedly connected with the mixing box, a rotating shaft is connected to the inner wall of one side of the mixing box in a rotating manner, a ball milling cylinder is fixedly connected to one end of the rotating shaft, an L-shaped motor base is fixedly connected to the outer wall of the other side of the mixing box, a driving motor is fixedly connected to the motor base, the output end of the driving motor penetrates through the outer wall of the mixing box and extends to be fixedly connected with the ball milling cylinder, a feeding pipe is communicated with the middle of the top end of the mixing box, the top end of the feeding pipe is in threaded connection with a matched feeding sealing cover, a feeding pipe is communicated with the middle of the top end of the ball milling cylinder, and a, the inside packing of ball mill section of thick bamboo has a plurality of balls, set up the multiunit on the outer wall of ball mill section of thick bamboo and be annular evenly distributed's ejection of compact micropore, the intercommunication has the inlet tube on the top outer wall of mixing box.
Further, the inlet pipe is located throws the material pipe under, throw fixedly connected with gangbar on the inner wall of the sealed lid of material, the one end of gangbar runs through throw the material pipe and extend to with the sealed fixed connection that covers of feeding, throw the handle bar of the sealed top fixedly connected with T font of material lid, through throwing the material pipe, throw the sealed lid of material, inlet pipe, the sealed lid of feeding, gangbar, handle bar's setting, during the use, the sealed lid of material is thrown off in the rotatory untwisting of accessible handle bar, under the linkage effect of gangbar, the sealed lid of feeding is twisted down simultaneously, can once throw in the material through throwing material pipe, inlet pipe in to the ball mill section of thick bamboo, is convenient for throw in the material, has improved the convenience, and after throwing in, twists again and throw the sealed lid of material and feeding, can prevent that the in-process.
Further, a plurality of connecting rods of bottom fixed connection of ball mill section of thick bamboo, the connecting rod is kept away from the one end fixedly connected with stirring vane of ball mill section of thick bamboo, through pivot, ball mill section of thick bamboo, motor base, driving motor, the ball, the setting of ejection of compact micropore, cladding agent, iron oxide yellow, clear water put in after finishing, start driving motor and can drive ball mill section of thick bamboo and carry out high-speed rotation, and then smash and preliminary mix cladding agent, iron oxide yellow, the cladding agent after smashing, iron oxide yellow powder can be got rid of to the mixing box through ejection of compact micropore, under the combined setting of connecting rod, stirring vane, the rotation of ball mill section of thick bamboo, accessible connecting rod drives stirring vane and rotates, and then stirs cladding agent, iron oxide yellow powder and clear water, make the three carry out further mixture, thereby in kibbling in-process, the mixture of material carries out in step, resources have been saved, The efficiency is improved.
Furthermore, the middle part of the bottom end of the mixing box is communicated with a material guide pipe, the inner wall of the bottom end of the mixing box is conical, the other end of the material guide pipe penetrates through the outer wall of the top of the dispersing box and extends into the dispersing box, the outer wall of one side of the dispersing box is fixedly connected with an ultrasonic generator, the inner wall of the bottom of the dispersing box is fixedly connected with a plurality of ultrasonic transducers, the outer wall of the other side of the dispersing box is communicated with a material discharge pipe, the ultrasonic transducers are all connected with the ultrasonic generator in a matching way, valves are arranged on the material guide pipe and the material discharge pipe, and after the materials are crushed and mixed, the valves on the material guide pipe are opened to guide the materials into the dispersing box, and then the ultrasonic generator and the ultrasonic transducers are started to carry out ultrasonic dispersion treatment on the materials, thereby collect crushing, mix, ultrasonic dispersion and handle as an organic whole, increased substantially material processing apparatus's rate of equipment utilization, the effectual area that has reduced equipment.
Further, the mole ratio of calcium carbonate, the organic silicon modified resin and the ferrous chloride in S1 is as follows: 1.2: 0.8: 1.
furthermore, the organic silicon modified resin in the S1 is one of alkyd resin, polyvinyl acetate resin, epoxy resin, acrylic resin, polyurethane resin and phenolic resin, and the organic silicon modified resin can effectively improve the heat resistance of the iron oxide yellow, and meanwhile, the organic silicon modified resin has the characteristics of corrosion resistance and oxidation resistance, can adapt to the preparation environment of the iron oxide yellow, cannot be damaged in the preparation process, and is beneficial to saving the cost by adopting calcium carbonate to replace sodium hydroxide.
Further, the coating agent in the S4 comprises 0.4-0.6 part by weight of a dispersing agent, 3-4 parts by weight of boric acid and 8-10 parts by weight of refractory soil, the weight of the iron oxide yellow in the S5 is three-fourths of the weight of the coating agent, and the liquid level of the clear water added into the mixing box in the S6 needs to exceed the bottom end of the ball milling barrel.
Further, the dispersing agent is a mixture of stearamide and higher alcohol, wherein the mass ratio of the stearamide to the higher alcohol is 58: 42, the prepared iron oxide yellow can be subjected to surface coating through reasonable design of the components and the mass ratio of the coating agent, design of a combined process method and arrangement of a material treatment device, so that the heat resistance is further improved, and the application range of the iron oxide yellow is greatly enlarged.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) in the scheme, the organic silicon modified resin is creatively selected and added in the preparation process of the ferrous oxide, has the characteristics of corrosion resistance, oxidation resistance and high temperature resistance, can adapt to the preparation environment of the iron oxide yellow, cannot be damaged, can effectively improve the heat resistance of the iron oxide yellow, adopts calcium carbonate to replace sodium hydroxide, is favorable for saving cost, can carry out surface coating on the prepared iron oxide yellow through reasonable design of components and mass ratio of a coating agent, design of a parallel combination process method and arrangement of a material treatment device, further improves the heat resistance, greatly improves the application range of the iron oxide yellow, can synchronously mix materials in the crushing process of the material treatment device, saves resources, improves the efficiency, and can carry out ultrasonic dispersion treatment on the materials, thereby integrating crushing, oxidation resistance and high temperature resistance, Mixing and ultrasonic dispersion treatment are integrated, the equipment utilization rate of the material treatment device is greatly improved, and the occupied area of the equipment is effectively reduced.
(2) Through throwing the material pipe, throw the sealed lid of material, the inlet pipe, the sealed lid of feeding, the gangbar, the setting of handle bar, during the use, the sealed lid of throwing the material is twisted off to the accessible handle bar rotation, under the linkage effect of gangbar, twist the sealed lid of feeding simultaneously off, can once throw the material pipe, the inlet pipe is to throwing in the material in the ball mill section of thick bamboo, be convenient for throw in the material, the convenience has been improved, and throw in the back that finishes, twist again and throw the sealed lid of material and feeding, can prevent that the in-process of material processing from taking place to.
(3) Through the pivot, a ball mill section of thick bamboo, the motor base, driving motor, the ball, ejection of compact micropore's setting, the cladding agent, iron oxide yellow, the clear water is put in and is accomplished the back, it can drive a ball mill section of thick bamboo and carry out high-speed rotation to start driving motor, and then to the cladding agent, iron oxide yellow is smashed and preliminary mixture, cladding agent after smashing, iron oxide yellow powder can be got rid of to the mixing box through ejection of compact micropore, at the connecting rod, stirring vane's joint sets up down, the rotation of a ball mill section of thick bamboo, the accessible connecting rod drives stirring vane and rotates, and then mix the cladding agent, iron oxide yellow powder and clear water, make the three carry out further mixture, thereby at kibbling in-process, carry out the mixture of material in step, resources are saved, efficiency is improved.
(4) Through the setting of passage, dispersion case, supersonic generator, ultrasonic transducer, after comminuted, the mixture finishes, open the valve on the passage, can be with the leading-in dispersion incasement of material, then start supersonic generator and ultrasonic transducer and can carry out ultrasonic dispersion to the material and handle to the collection is smashed, is mixed, ultrasonic dispersion handles as an organic whole, has increased substantially material processing apparatus's rate of equipment utilization, the effectual area that reduces equipment.
(5) The organic silicon modified resin can effectively improve the heat resistance of the iron oxide yellow, has the characteristics of corrosion resistance and oxidation resistance, can adapt to the preparation environment of the iron oxide yellow, cannot be damaged in the preparation process, adopts calcium carbonate to replace sodium hydroxide, and is favorable for saving the cost.
(6) Through reasonable design of the components and the mass ratio of the coating agent, design of a combined process method and arrangement of a material processing device, the prepared iron oxide yellow can be subjected to surface coating, the heat resistance is further improved, and the application range of the iron oxide yellow is greatly improved.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a front view of the material handling apparatus of the present invention;
FIG. 3 is a cross-sectional view of the interior of the mixing box of the present invention;
FIG. 4 is an enlarged view taken at A of FIG. 3 in accordance with the present invention;
FIG. 5 is a cross-sectional view of the interior of the ball mill cartridge of the present invention;
fig. 6 is a cross-sectional view of the interior of the dispersion box of the present invention.
The reference numbers in the figures illustrate:
101. a mixing box; 102. a rotating shaft; 103. a ball milling cylinder; 104. a motor base; 105. a drive motor; 106. a feeding pipe; 107. a feeding sealing cover; 108. a feed pipe; 109. a feeding sealing cover; 110. a linkage rod; 111. a handle bar; 112. grinding balls; 113. discharging micropores; 114. a water inlet pipe; 115. a connecting rod; 116. a stirring blade; 117. a material guide pipe; 201. a dispersion box; 202. a support bar; 203. an ultrasonic generator; 204. an ultrasonic transducer; 205. a discharge pipe.
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. 1-6, a process for producing heat-resistant yellow iron oxide includes the following steps:
s1, mixing the raw materials: adding a proper amount of calcium carbonate, organic silicon modified resin and water into a reaction kettle, introducing air and stirring, and then adding a corresponding amount of ferrous chloride into the reaction kettle;
s2, oxidation: adjusting the temperature of the reaction kettle to 85-90 ℃, continuously blowing air into the reaction kettle in the process until the required color is obtained, preserving the heat for 45-65min, and discharging;
s3, impurity removal and subsequent treatment: after discharging, adding a dilute hydrochloric acid solution to remove redundant calcium carbonate, and then rinsing, filter pressing, drying and crushing to obtain iron oxide yellow containing the organic silicon modified resin;
s4, adding a coating agent: weighing a proper amount of coating agent, putting the coating agent into a ball milling cylinder 103 of a material processing device, weighing the iron oxide yellow prepared in the corresponding amount S3, and putting the iron oxide yellow into the ball milling cylinder 103 in the same way;
s5, material processing: injecting a proper amount of clear water into the mixing box 101 through a water inlet pipe 114, starting a driving motor 105, driving a ball milling cylinder 103 to rotate, carrying out ball milling and stirring mixing treatment on a coating agent and iron oxide yellow, obtaining a preliminary mixture after 2 hours, closing a motor base 104, opening a valve on a material guide pipe 117, guiding the preliminary mixture into a dispersion box 201, carrying out ultrasonic dispersion treatment on the preliminary mixture, treating for 3 hours to obtain a final mixture, and discharging the final mixture through a material discharge pipe 205;
s6, neutralizing and aging: slowly dropwise adding ethyl acetate into the final mixture in the S5 while stirring until the pH value of the mixed solution is neutral, and then standing and aging;
s7, solid-liquid separation: and (4) centrifugally separating the aged mixed solution in the S6, wet-grinding the solid material by using a three-roll grinder, and drying to obtain the iron oxide yellow with the surface coated with the oil-containing organic silicon modified resin.
The mol ratio of the calcium carbonate, the organic silicon modified resin and the ferrous chloride in S1 is as follows: 1.2: 0.8: 1, the organic silicon modified resin in the S1 is one of alkyd resin, polyvinyl resin, epoxy resin, acrylic resin, polyurethane resin and phenolic resin, the organic silicon modified resin can effectively improve the heat resistance of iron oxide yellow, and meanwhile, the organic silicon modified resin has the characteristics of corrosion resistance and oxidation resistance, can adapt to the preparation environment of the iron oxide yellow and cannot be damaged in the preparation process, the coating agent in the S5 comprises 0.4-0.6 part by weight of a dispersing agent, 3-4 parts by weight of boric acid and 8-10 parts by weight of refractory soil, the weight of the iron oxide yellow in the S4 is three quarters of the weight of the coating agent, the liquid level of clear water added into the mixing box 101 in the S6 does not pass through the bottom end of the ball milling barrel 103, the dispersing agent is a mixture of stearamide and higher alcohol, wherein the mass ratio of the stearamide to the higher alcohol is 58: 42, the prepared iron oxide yellow can be subjected to surface coating through reasonable design of the components and the mass ratio of the coating agent, design of a combined process method and arrangement of a material treatment device, so that the heat resistance is further improved, and the application range of the iron oxide yellow is greatly enlarged.
Referring to fig. 2-5, the material processing apparatus in S4 includes a mixing box 101 and a dispersing box 201 disposed below the mixing box 101, two symmetrically disposed support rods 202 are fixedly connected to the top end of the dispersing box 201, the top ends of the support rods 202 are fixedly connected to the mixing box 101, a rotating shaft 102 is rotatably connected to the inner wall of one side of the mixing box 101, a ball milling cylinder 103 is fixedly connected to one end of the rotating shaft 102, an L-shaped motor base 104 is fixedly connected to the outer wall of the other side of the mixing box 101, a driving motor 105 is fixedly connected to the motor base 104, the output end of the driving motor 105 penetrates through the outer wall of the mixing box 101 and extends to be fixedly connected to the ball milling cylinder 103, a feeding pipe 106 is connected to the middle of the top end of the mixing box 101, a matched feeding sealing cover 107 is threadedly connected to the top end of the feeding pipe 106, a feeding pipe 108 is communicated to the middle of the top end of the, the interior of the ball milling cylinder 103 is filled with a plurality of milling balls 112, the outer wall of the ball milling cylinder 103 is provided with a plurality of groups of discharge micropores 113 which are uniformly distributed in an annular shape, the outer wall of the top of the mixing box 101 is communicated with a water inlet pipe 114, the feed pipe 108 is positioned under the feeding pipe 106, the inner wall of the feeding sealing cover 107 is fixedly connected with a linkage rod 110, one end of the linkage rod 110 penetrates through the feeding pipe 106 and extends to be fixedly connected with the feeding sealing cover 109, the top end of the feeding sealing cover 107 is fixedly connected with a T-shaped handle rod 111, and through the arrangement of the feeding pipe 106, the feeding sealing cover 107, the feed pipe 108, the feeding sealing cover 109, the linkage rod 110 and the handle rod 111, when in use, the feeding sealing cover 107 can be screwed off through the handle rod 111 in a rotating manner, and under the linkage effect of the linkage rod 110, the feeding sealing cover 109 is simultaneously screwed off, so that materials can, the material feeding is convenient, the convenience is improved, after the material feeding is finished, the material feeding sealing cover 107 and the material feeding sealing cover 109 are screwed again, the leakage in the material processing process can be prevented, the bottom end of the ball grinding cylinder 103 is fixedly connected with a plurality of connecting rods 115, one end of each connecting rod 115, which is far away from the ball grinding cylinder 103, is fixedly connected with a stirring blade 116, through the arrangement of the rotating shaft 102, the ball grinding cylinder 103, the motor base 104, the driving motor 105, the grinding balls 112 and the discharging micropores 113, after the coating agent, the iron oxide yellow and the clean water are fed, the driving motor 105 is started to drive the ball grinding cylinder 103 to rotate at high speed, further the coating agent and the iron oxide yellow are crushed and preliminarily mixed, the crushed coating agent and the iron oxide yellow powder can be thrown into the mixing box 101 through the discharging micropores 113, under the combined arrangement of the connecting rods 115 and the stirring blades 116, the rotation of the ball grinding cylinder 103 can drive the stirring blades 116 to rotate through the, and then the coating agent, the iron oxide yellow powder and the clear water are stirred to further mix the coating agent, the iron oxide yellow powder and the clear water, so that the materials are synchronously mixed in the crushing process, the resources are saved, and the efficiency is improved.
Referring to fig. 2 and 6, a material guiding pipe 117 is communicated with the middle of the bottom end of the mixing box 101, the inner wall of the bottom end of the mixing box 101 is tapered, the other end of the material guiding pipe 117 penetrates through the outer wall of the top of the dispersing box 201 and extends into the dispersing box 201, an ultrasonic generator 203 is fixedly connected to the outer wall of one side of the dispersing box 201, a plurality of ultrasonic transducers 204 are fixedly connected to the inner wall of the bottom of the dispersing box 201, a material discharging pipe 205 is communicated with the outer wall of the other side of the dispersing box 201, the plurality of ultrasonic transducers 204 are all connected with the ultrasonic generator 203 in a matching manner, valves are arranged on the material guiding pipe 117 and the material discharging pipe 205, and after the materials are crushed and mixed, the valves on the material guiding pipe 117 are opened to guide the materials into the dispersing box 201, and then the ultrasonic generator 203 and the ultrasonic transducers 204 are started to perform ultrasonic dispersion treatment on the materials, thereby collect crushing, mix, ultrasonic dispersion and handle as an organic whole, increased substantially material processing apparatus's rate of equipment utilization, the effectual area that has reduced equipment.
In the preparation process of the ferrous oxide, the organic silicon modified resin is creatively selected and added, has the characteristics of corrosion resistance, oxidation resistance and high temperature resistance, can adapt to the preparation environment of the iron oxide yellow, cannot be damaged, can effectively improve the heat resistance of the iron oxide yellow, adopts calcium carbonate to replace sodium hydroxide, is favorable for saving cost, can carry out surface coating on the prepared iron oxide yellow by reasonably designing the components and the mass ratio of a coating agent, designing a parallel combination process method and arranging a material treatment device, further improves the heat resistance, greatly improves the application range of the iron oxide yellow, can synchronously mix materials in the crushing process of the material treatment device, saves resources, improves the efficiency, and can carry out ultrasonic dispersion treatment on the materials, thereby integrating crushing, oxidation resistance and high temperature resistance, Mixing and ultrasonic dispersion treatment are integrated, the equipment utilization rate of the material treatment device is greatly improved, and the occupied area of the equipment is effectively reduced.
The foregoing is only a preferred embodiment 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 (9)

1. A production process of heat-resistant iron oxide yellow is characterized by comprising the following steps: the method comprises the following steps:
s1, mixing the raw materials: adding a proper amount of calcium carbonate, organic silicon modified resin and water into a reaction kettle, introducing air and stirring, and then adding a corresponding amount of ferrous chloride into the reaction kettle;
s2, oxidation: adjusting the temperature of the reaction kettle to 85-90 ℃, continuously blowing air into the reaction kettle in the process until the required color is obtained, preserving the heat for 45-65min, and discharging;
s3, impurity removal and subsequent treatment: after discharging, adding a dilute hydrochloric acid solution to remove redundant calcium carbonate, and then rinsing, filter pressing, drying and crushing to obtain iron oxide yellow containing the organic silicon modified resin;
s4, adding a coating agent: weighing a proper amount of coating agent, putting the coating agent into a ball milling cylinder (103) of a material processing device, weighing the iron oxide yellow prepared in the corresponding amount S3, and putting the iron oxide yellow into the ball milling cylinder (103) in the same way;
s5, material processing: injecting a proper amount of clear water into a mixing box (101) through a water inlet pipe (114), starting a driving motor (105), driving a ball milling cylinder (103) to rotate, carrying out ball milling and stirring mixing treatment on a coating agent and iron oxide yellow, obtaining a primary mixture after 2 hours, closing a motor base (104), opening a valve on a material guide pipe (117), guiding the primary mixture into a dispersion box (201), carrying out ultrasonic dispersion treatment on the primary mixture, treating for 3 hours to obtain a final mixture, and discharging the final mixture through a material discharge pipe (205);
s6, neutralizing and aging: slowly dropwise adding ethyl acetate into the final mixture in the S5 while stirring until the pH value of the mixed solution is neutral, and then standing and aging;
s7, solid-liquid separation: and (4) centrifugally separating the aged mixed solution in the S6, wet-grinding the solid material by using a three-roll grinder, and drying to obtain the iron oxide yellow with the surface coated with the oil-containing organic silicon modified resin.
2. The process for producing heat-resistant yellow iron oxide according to claim 1, wherein: the material processing device in the S (4) comprises a mixing box (101) and a dispersing box (201) arranged below the mixing box (101), wherein two symmetrically arranged support rods (202) are fixedly connected to the top end of the dispersing box (201), the top ends of the support rods (202) are fixedly connected with the mixing box (101), a rotating shaft (102) is connected to the inner wall of one side of the mixing box (101) in a rotating mode, a ball milling barrel (103) is fixedly connected to one end of the rotating shaft (102), an L-shaped motor base (104) is fixedly connected to the outer wall of the other side of the mixing box (101), a driving motor (105) is fixedly connected to the motor base (104), the output end of the driving motor (105) penetrates through the outer wall of the mixing box (101) and extends to be fixedly connected with the ball milling barrel (103), and a feeding pipe (106) is communicated with the middle of the top end of the mixing box (101), the material feeding device is characterized in that the top end of the material feeding pipe (106) is in threaded connection with a material feeding sealing cover (107) matched with the top end of the material feeding pipe, the middle of the top end of the ball grinding cylinder (103) is communicated with the material feeding pipe (108), the top end of the material feeding pipe (108) is in threaded connection with a material feeding sealing cover (109) matched with the top end of the material feeding pipe, a plurality of grinding balls (112) are filled in the ball grinding cylinder (103), a plurality of groups of discharging micropores (113) which are uniformly distributed in an annular shape are formed in the outer wall of the ball grinding cylinder (103), and the top outer wall.
3. The process for producing heat-resistant yellow iron oxide according to claim 2, wherein: the feeding pipe (108) is located under the feeding pipe (106), a linkage rod (110) is fixedly connected to the inner wall of the feeding sealing cover (107), one end of the linkage rod (110) penetrates through the feeding pipe (106) and extends to be fixedly connected with the feeding sealing cover (109), and a T-shaped handle rod (111) is fixedly connected to the top end of the feeding sealing cover (107).
4. The process for producing heat-resistant yellow iron oxide according to claim 2, wherein: the bottom end of the ball milling barrel (103) is fixedly connected with a plurality of connecting rods (115), and one end, far away from the ball milling barrel (103), of each connecting rod (115) is fixedly connected with a stirring blade (116).
5. The process for producing heat-resistant yellow iron oxide according to claim 2, wherein: the middle part intercommunication of mixing box (101) bottom has passage (117), the bottom inner wall of mixing box (101) sets up to the toper, the other end of passage (117) runs through the top outer wall of dispersion case (201) and extends to dispersion case (201) inside, fixedly connected with supersonic generator (203) on the outer wall of dispersion case (201) one side, a plurality of ultrasonic transducer (204) of fixedly connected with on the bottom inner wall of dispersion case (201), the intercommunication has row material pipe (205) on the outer wall of dispersion case (201) opposite side, and is a plurality of ultrasonic transducer (204) all with supersonic generator (203) accordant connection, all be provided with the valve on passage (117), row material pipe (205).
6. The process for producing heat-resistant yellow iron oxide according to claim 1, wherein: the mol ratio of the calcium carbonate, the organic silicon modified resin and the ferrous chloride in the S1 is as follows: 1.2: 0.8: 1.
7. the process for producing heat-resistant yellow iron oxide according to claim 1, wherein: the organic silicon modified resin in the S1 is one of alkyd resin, polyvinyl acetate resin, epoxy resin, acrylic resin, polyurethane resin and phenolic resin.
8. The process for producing heat-resistant yellow iron oxide according to claim 1, wherein: the coating agent in the S4 comprises 0.4-0.6 part by weight of a dispersing agent, 3-4 parts by weight of boric acid and 8-10 parts by weight of refractory soil, the weight of the iron oxide yellow in the S5 is three-fourths of the weight of the coating agent, and the liquid level of clear water added into the mixing box (101) in the S6 needs to exceed the bottom end of the ball milling cylinder (103).
9. The process for producing heat-resistant yellow iron oxide according to claim 8, wherein: the dispersing agent is a mixture of stearamide and higher alcohol, wherein the mass ratio of the stearamide to the higher alcohol is 58: 42.
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DE3670304D1 (en) * 1985-11-06 1990-05-17 Bayer Ag HEAT-RESISTANT YELLOW PIGMENTS, METHOD FOR THE PRODUCTION AND USE THEREOF.
JPH1112491A (en) * 1997-06-23 1999-01-19 Toda Kogyo Corp Production of heat-resistant yellow hydrated iron oxide pigment
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