CN111960475A - Preparation process of high-pigment iron oxide yellow - Google Patents
Preparation process of high-pigment iron oxide yellow Download PDFInfo
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- CN111960475A CN111960475A CN202010871194.8A CN202010871194A CN111960475A CN 111960475 A CN111960475 A CN 111960475A CN 202010871194 A CN202010871194 A CN 202010871194A CN 111960475 A CN111960475 A CN 111960475A
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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Abstract
The invention discloses a preparation process of high-pigment iron oxide yellow, and belongs to the technical field of pigment preparation. The invention adopts the measures of controlling refinement, self-making ferrous sulfate and the like to control the probability of heavy metal participating in oxidation in the production process by preparing the seed crystal and preparing the high-pigment iron oxide yellow, simultaneously utilizes a special oxidation cylinder to ensure that an oxidation medium reacts uniformly, avoids using harmful substances, simultaneously precisely controls the reaction temperature and the concentration of the medium, ensures that the generated iron oxide yellow particle particles are uniformly in a needle shape, and controls the length-diameter ratio of the particles to be 1:2, the produced iron oxide yellow particles are soft and have strong tinting strength.
Description
Technical Field
The invention relates to the technical field of pigment preparation, in particular to a preparation process of high-pigment iron oxide yellow.
Background
The iron oxide yellow contains iron oxide as main component and has chemical formula of Fe2O3·H2O, is the monohydrate of iron oxide. The iron oxide yellow pigment is used as pigment or colorant for prefabricated parts and building products in various concrete, is also suitable for coloring and protecting various coatings, can also be used for toy paint, decorative paint, furniture paint, electrophoretic paint and enamel paint, and is also suitable for coloring plastic products and rubber products. And can also be used as an intermediate of iron oxide pigments, such as iron oxide red, iron oxide black, etc. In addition, the iron oxide yellow pigment can also be used for various cosmetics, paper,And (4) coloring the leather.
When the iron oxide yellow is mainly used for coloring tipping paper of filter-tipped cigarettes and children toys, strict requirements are imposed on high coloring power of the iron oxide yellow, and meanwhile, strict requirements are imposed on the heavy metal content in the iron oxide yellow and the limitation of harmful substances harmful to human bodies.
CN202010221641.5 provides a heat-resistant iron oxide yellow with high tinting strength, a preparation method and an application thereof, wherein the preparation method comprises the following steps: and sequentially coating the surface of the iron oxide yellow to be treated with soluble zinc salt and soluble aluminum salt. The iron oxide yellow to be treated comprises the iron oxide yellow after Pennismann reaction or precipitation reaction. The method is simple and convenient to operate, environment-friendly and safe, and the prepared heat-resistant iron oxide yellow is heat-resistant and good in tinting strength and dispersibility, but other heavy metal salts are introduced into the iron oxide yellow, so that the iron oxide yellow has certain limitation on products directly used for human bodies.
Therefore, it is necessary to provide a preparation process of high-pigment yellow iron oxide, so as to solve the problems of the prior art that the content of heavy metals and the content of harmful substances are too high.
Disclosure of Invention
The invention aims to provide a preparation process of high-pigment iron oxide yellow, which aims to solve the problem that a non-toxic inorganic pigment replaces an organic pigment with high tinting strength, and the application field is expanded to the edible field; the content of heavy metals in the prepared iron oxide yellow is reduced to the minimum, even avoided; and also reduces the residue of harmful substances harmful to human body.
In order to solve the technical problems, the invention adopts the following technical scheme:
on one hand, the invention provides a preparation process of high-pigment iron oxide yellow, which comprises the following steps:
the method comprises the following steps: the seed crystal is prepared by the following steps of,
adding clear water into the barrel, adding sulfuric acid, introducing air, and stirring to obtain dilute sulfuric acid;
adding a ferrous sulfate solution into the seed crystal barrel, supplementing clear water, introducing air and stirring to ensure that the concentration of the ferrous sulfate in the barrel is about 21g/100ml-23g/100ml and the pH value is 3-4;
adding dilute alkali liquor, closing down the air quantity, adding dilute alkali liquor or adding a small amount of clear water to ensure the reaction volume;
detecting in the reaction process, and stopping the reaction if the seed crystal requirement is met;
if the seed crystal is oxidized for 4 to 9 hours and the gel is formed, increasing the air amount for reaction;
oxidizing the seed crystal for 15-25 hours, and then converting the color into earthy yellow to obtain the end point;
immediately stopping introducing air for oxidation after the end point is reached, sampling 50ml, and placing the sample in a colorimetric tube for detecting the quality of the seed crystal;
step two preparation of high-pigment iron oxide yellow
Cleaning the oxidation barrel; removing the bronchus, dredging and cleaning; if residual iron sheet remains in the previous experiment, loosening, cleaning and dedusting are needed; uniformly putting the iron sheet with the impurities removed and the rust reduced into the barrel, and uniformly matching the thickness, thinness, excellence and inferiority of the iron sheet;
putting seed crystals, adding clear water, starting a small amount of air, uniformly stirring, and detecting the concentration of the opened barrel;
heating to 75 ℃ within 8 hours, controlling the temperature to be 75-81 ℃ within 24 hours, and controlling the temperature to be 81-89 ℃ after 24 hours; when the concentration is lower in the middle of the reaction, a proper amount of ferrous sulfate, namely seed crystals, is added in emergency;
and (3) starting sampling and colorimetric after about 50 hours of reaction, recording the color condition, and carrying out colorimetric 1-2 times every 6-8 hours when the end point is approached, wherein the color is compared with a barreled standard sample: reaching the end point of approximation, micro or slight brightness;
and after the color reaches the end point, immediately closing the air valve, opening the reaction barrel, simultaneously sampling and detecting the barrel release concentration and yield, and completing barrel release within 3 hours.
Further, in the first step, the concentration of the ferrous sulfate solution is controlled to be 35-50g/100ml, and the pH value is controlled to be 4-6.
Further, in the first step, the concentration of the liquid caustic soda is 30% by mass fraction. The liquid alkali is sodium hydroxide solution, potassium hydroxide solution and the like.
Further, in the step one, the air is introducedThe amount is 150-200m3Hour/hour; the amount of the shut-down air is 70-90m3In terms of hours.
Further, in the step one, the detecting the seed crystal requirement is: the pH value is 4-6, the residual iron is 10.00-14.00g/100ml, and the solid content is more than or equal to 3.5g/100 ml.
Further, in the step one, the air quantity increasing inlet quantity is 150-3In terms of hours.
Further, the seed crystal preparation process is as follows:
1) collecting 3400kg-4500kg ferrous sulfate solution, controlling concentration at 35-50g/100ml, pH 4-6, temperature (normal temperature) below 37 deg.C, and color light green;
2) measuring 1200kg of liquid caustic soda with the concentration of 30%, and compressing and conveying the liquid caustic soda into a dilute caustic soda tank by using air;
3) cleaning the seed crystal barrel, and checking whether an air pipeline and a bottom valve of the seed crystal barrel are normal;
4) adding 1000ml-5000ml of clear water into the barrel, adding 100ml of sulfuric acid, introducing air and stirring uniformly;
5) adding ferrous sulfate solution, supplementing clear water, and stirring with air for 2 min to make the ferrous sulfate concentration in the barrel about 21g/100ml-23g/100ml and pH value 3-4;
6) air (150-3Per hour), opening a dilution water valve, slowly adding dilute alkali liquor, and controlling the adding within 5-10 minutes;
7) after the alkali addition is finished, the air quantity is cut off (70-90 m)3Hour), adding dilute alkali solution or adding a small amount of clear water to ensure that the reaction volume is 24m3；
8) Detecting in the reaction process, and stopping the reaction if the seed crystal requirement is met; if the seed crystal is oxidized for 4-9 hours and the gel is formed, the air amount is increased to 150-200m3Hour/hour;
9) oxidizing the seed crystal for 15-25 hours, and then converting the color into earthy yellow (similar to a standard sample) to obtain an end point;
10) immediately stopping introducing air for oxidation after the end point is reached, sampling 50ml, and placing the sample in a colorimetric tube for detecting the quality of the seed crystal; the pH value of the seed crystal is required to be 4-6, the residual iron is 10.00-14.00g/100ml, and the solid content is more than or equal to 3.5g/100 ml.
Further, in the second step, the concentration of the barrel opening is 4.0g/100ml-6.0g/100 ml.
Further, in the second step, the air amount is 70-90m before the temperature reaches 75 ℃ within 8 hours3The seed crystal is prevented from being continuously oxidized in one hour; after the temperature is raised to 75 ℃, the air amount is 150-3And (4) turning the air in the barrel uniformly every hour.
Furthermore, in the second step, the temperature is controlled to be between 81 and 89 ℃, the concentration in the middle of the reaction is lower than 4.0g/100ml to 6.0g/100ml, and the seed crystal is added in case of emergency.
Further, the preparation process of the high-pigment iron oxide yellow comprises the following specific steps:
step one preparation of seed crystals
1) Collecting 3400kg-4500kg ferrous sulfate solution, controlling concentration at 35-50g/100ml, pH 4-6, temperature (normal temperature) below 37 deg.C, and color light green;
2) measuring 1200kg of liquid caustic soda with the concentration of 30%, and compressing and conveying the liquid caustic soda into a dilute caustic soda tank by using air;
3) cleaning the seed crystal barrel, and checking whether an air pipeline and a bottom valve of the seed crystal barrel are normal;
4) adding 1000ml-5000ml of clear water into the barrel, adding 100ml of sulfuric acid, introducing air and stirring uniformly;
5) adding ferrous sulfate solution, supplementing clear water, and stirring with air for 2 min to make the ferrous sulfate concentration in the barrel about 21g/100ml-23g/100ml and pH value 3-4;
6) air (150-3Per hour), opening a dilution water valve, slowly adding dilute alkali liquor, and controlling the adding within 5-10 minutes;
7) after the alkali addition is finished, the air quantity is cut off (70-90 m)3Hour), adding dilute alkali solution or adding a small amount of clear water to ensure that the reaction volume is 24m3(ii) a 8) Detecting in the reaction process, and stopping the reaction if the seed crystal requirement is met; if the seed crystal is oxidized for 4-9 hours and the gel is formed, the air amount is increased to 150-200m3Hour/hour;
9) oxidizing the seed crystal for 15-25 hours, and then converting the color into earthy yellow (similar to a standard sample) to obtain an end point;
10) immediately stopping introducing air for oxidation after the end point is reached, sampling 50ml, and placing the sample in a colorimetric tube for detecting the quality of the seed crystal; the pH value of the seed crystal is required to be 4-6, the residual iron is 10.00-14.00g/100ml, and the solid content is more than or equal to 3.5g/100 ml;
step two preparation of high-pigment iron oxide yellow
11) Cleaning the oxidation barrel; removing the bronchus, dredging and cleaning; if residual iron sheet remains in the previous experiment, loosening, cleaning and dedusting are needed; uniformly putting the iron sheet with the impurities removed and the rust reduced into the barrel, and uniformly matching the thickness, thinness, excellence and inferiority of the iron sheet;
12) seed crystals are put in and clear water is added for about 12m3Ensure that the volume of the barrel opening reaches 32m3A small amount of air is turned on to stir uniformly and the concentration of the mixture in the barrel is measured (generally from 4.0g/100ml to 6.0g/100 ml).
13) The air quantity is as small as possible (70-90 m) before the temperature is raised to 75 ℃ within 8 hours and reaches 75 DEG C3Per hour) to prevent further oxidation of the seed; after the temperature is raised to 75 ℃, the air amount is increased (150- & ltwbr/& gt200 m)3Hour), the air is evenly stirred in the barrel; the temperature is controlled to be 75-81 ℃ within 24 hours, and after 24 hours, the temperature is controlled to be 81-89 ℃. When the concentration in the middle of the reaction is lower than 4.0g/100ml to 6.0g/100ml, a proper amount of ferrous sulfate, namely seed crystals, is added in emergency; controlling the reaction progress through the processes of reaction degree, reaction concentration and the like, so that the prepared iron oxide yellow ions are uniform and needle-shaped;
14) the color in the barrel is generally required to be sampled and compared within about 50 hours, the color condition is recorded, and when the color is close to the end point, the color is compared for 1-2 times per shift, and the color comparison operation procedure is required to be fast, accurate, timely and strictly maintained. Color comparison to bucket standards: reaching the end point of being similar, micro or slightly bright.
15) Barrel placing: and after the color reaches the end point, immediately closing the air valve, opening the reaction barrel, simultaneously sampling and detecting the barrel release concentration and yield, and completing barrel release within 3 hours.
The iron oxide yellow produced by the process is pure in color, strong in relative tinting strength and uniform in particles.
Compared with the prior art, the invention has the following beneficial effects:
(1) the iron oxide yellow prepared by the process has high purity, strong tinting strength and uniform particles. In the preparation process, the reaction time, the reaction concentration, the heating temperature and the air amount are strictly controlled, so that the properties of the prepared iron oxide yellow are ensured. The reaction rate is controlled by adjusting the air quantity, so that excessive oxidation is avoided; the subsequent preparation of the high-pigment iron oxide yellow is facilitated by controlling the standard of the seed crystal; the reaction progress is controlled by combining the reaction temperature with the air amount, so that the prepared iron oxide yellow is uniform and has strong tinting strength.
(2) The iron oxide yellow obtained by the preparation process of the high-pigment iron oxide yellow provided by the invention has low content of heavy metals such as cadmium, lead, mercury and hexavalent chromium, and has small residue of harmful substances, such as bromobenzene. A special oxidation barrel is adopted in the preparation process, and the cleaning and impurity removing processes are also carried out before the preparation; and heavy metals, organic harmful substances and the like are not introduced.
(3) The preparation process provided by the invention adopts measures of controlling refinement, self-making ferrous sulfate and the like to control the probability of heavy metal participating in oxidation in the production process, simultaneously utilizes a special oxidation cylinder to ensure that an oxidation medium reacts uniformly and avoid using harmful substances, and simultaneously precisely prepares to control the reaction temperature and the medium concentration to ensure that the generated iron oxide yellow particle particles are uniformly in a needle shape, and the needle shape length-diameter ratio of the particles is controlled to be 1:2, the produced iron oxide yellow particles are soft and have strong tinting strength.
Drawings
FIG. 1 is an electron microscope comparison of a product (b) produced in example 1 with a conventional product (a); it is obvious from the 50000 times magnified electron micrograph of figure (a) that the common iron oxide yellow has a large amount of small particles and a wide particle size distribution range; as can be seen from the 50000 times magnified electron micrograph in the figure (b), the iron oxide yellow prepared by the preparation process provided by the invention has uniform particle size distribution and relatively consistent length-diameter ratio.
FIG. 2 is a graph showing the results of measuring the contents of harmful substances and heavy metals in the product produced in example 1. As can be seen from the results of the graph, the heavy metal content therein was not detected; harmful substances polybrominated biphenyls and polybrominated diphenyl ethers were not detected.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
The preparation process of the high-pigment iron oxide yellow provided by the embodiment comprises the following specific steps:
step one preparation of seed crystals
1. Preparation work
1.1 detecting the concentration, pH value, temperature, color and the like of ferrous sulfate, and recording, wherein the requirements are as follows:
ferrous sulfate concentration (FeSO)4.7H2O) is 35-50g/100ml, pH value is 4-6, temperature (normal temperature) is lower than 37 ℃, and color is light green.
1.2 calculating ferrous sulfate 3400kg-4500kg (100% FeSO) in ferrous sulfate storage tank4.7H2O) height to be measured.
1.3 measuring 1200kg of 30 percent liquid caustic soda 750-.
1.4 cleaning the seed crystal barrel, and checking whether the air pipeline and the bottom valve of the seed crystal barrel are normal.
2. Operation of
2.1 metering in clear water until the identification of vacancy in the barrel is standard, adding 100ml of sulfuric acid and adding air and stirring uniformly.
2.2 after the ferrous sulfate is metered, adding clear water to enable the liquid level in the barrel to rise to the specified scale, namely, the vacancy is 3.5 meters, stirring for 2 minutes by using air, detecting, requiring the dilution concentration to be about 21g/100ml-23g/100ml and the pH value to be 3-4, simultaneously recording the temperature before neutralization, and making an original record.
2.3 introducing air (150-3And/hour), opening a dilution water valve, slowly adding the dilute alkali liquor, and controlling the adding to be finished within 5-10 minutes.
2.4 after the addition of the base, the amount of air (70-90 m) was reduced3One hour), adding alkali and adding a small amount of clear water, controlling the reaction liquid level at a specified scale, controlling the reaction liquid level to be 2.8 meters in vacant position, and ensuring the reaction volume to be 24m3. Adding clear water after thickening in summer and leaving more than 0.5 m of vacant site) and entering seed crystal oxidation by taking a ruler on a barrel as a standard.
2.5 the sampling detection by the central controller is that the residual iron is 10.00-14.00 percent and the pH value is 4-6.
2.6 seed crystal oxidation for 4-9 hours, the air amount is increased to 150-200m3In terms of hours.
2.7 oxidizing the seed crystal for 15-25 h, and then converting the color into earthy yellow (similar to the standard sample) to obtain the end point.
2.8 after the end point, immediately stopping oxidation, sampling 50ml by a central controller, and placing the sample in a colorimetric tube to detect the seed crystal quality. The pH value is required to be 4-6, the residual iron is 10.00-14.00g/100ml, and the solid content is more than or equal to 3.5g/100 ml.
Step two preparation of high-pigment iron oxide yellow
1. Preparation work
1.1, cleaning the oxidation barrel, loosening the residual iron sheet, cleaning, removing dust, removing the bronchus, dredging and cleaning.
1.2, iron sheets with impurities removed and rust reduced are uniformly put into the barrel, and the iron sheets are uniformly matched in thickness, thinness, excellence and inferiority.
3 sampling and detecting the residual iron, pH value and color of the seed crystal and reserving the sample for future reference.
Operation of
2.1 about 12m of seed crystals (barrel)3Adding clear water to ensure that the volume of the barrel is up to 32m3) And after the temperature is raised to 24 hours, ensuring that the liquid level is 50-80cm away from the bung hole.
2.2 open a small amount of air to stir well and measure the open-barrel concentration (typically between 4.0g/100ml and 6.0g/100 ml).
2.3 temperature control: the temperature is increased to 75 ℃ within 8 hours, the temperature is controlled to be between 75 and 81 ℃ within 24 hours, and the temperature is controlled to be between 81 and 89 ℃ after 24 hours.
2.4 air quantity control: before 8 hours reach 75 ℃, the air quantity is as small as possible, and the seed crystal is prevented from being continuously oxidized; after the temperature is raised to 75 ℃, the air quantity is increased, so that the air is uniformly stirred in the barrel.
2.5 concentration control: after the seed crystal is transferred, the concentration of the seed crystal is maintained at 4.0g/100ml-6.0g/100ml, and when the concentration is low in the middle of the reaction, a proper amount of ferrous iron is added in emergency.
2.6 color control: the color in the barrel is generally required to be sampled and compared within about 50 hours, the color condition is recorded, and when the color is close to the end point, the color is compared for 1-2 times per shift, and the color comparison operation procedure is required to be fast, accurate, timely and strictly maintained. Color comparison to bucket standards: reaching the end point of being similar, micro or slightly bright.
2.7, barrel placing: and stopping steam and discharging the barrel immediately after the color reaches the end point, and sampling and detecting the concentration and yield of the barrel, wherein the barrel discharging is finished within 3 hours.
The iron oxide yellow produced by the process is pure in color, strong in relative tinting strength and uniform in particles.
And (3) detection test:
the test method comprises the following steps: with reference to IEC 62321-4:2013+ A1:2017, IEC 62321-5:2013, IEC 62321-7-2:2017, IEC 62321-6:2015 and IEC 62321-8:2017, analysis was performed using ICp-OES, UV-Vis and GC-MS. The results are shown in FIG. 2. Test sample No. 003, description: a yellow powder; wherein MDL represents the method detection limit; ND means not detected (< MDL); "-" indicates unspecified.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation process of high-pigment iron oxide yellow is characterized by comprising the following specific steps:
the method comprises the following steps: the seed crystal is prepared by the following steps of,
cleaning a cleaning barrel, adding clear water into the barrel, adding sulfuric acid, introducing air, and stirring uniformly to prepare dilute sulfuric acid;
adding a ferrous sulfate solution into the seed crystal barrel, supplementing clear water, introducing air, and stirring to ensure that the concentration of the ferrous sulfate in the barrel is about 21-23g/100ml and the pH value is 3-4;
adding dilute alkali liquor, closing down the air quantity, adding dilute alkali liquor or adding a small amount of clear water to ensure the reaction volume;
detecting in the reaction process, and stopping the reaction if the seed crystal requirement is met;
if the seed crystal is oxidized for 4 to 9 hours and the gel is formed, increasing the air amount for reaction;
oxidizing the seed crystal for 15-25 hours, and then converting the color into earthy yellow to obtain the end point;
immediately stopping introducing air for oxidation after the end point is reached, sampling 50ml, and placing the sample in a colorimetric tube for detecting the quality of the seed crystal;
step two preparation of high-pigment iron oxide yellow
Cleaning the oxidation barrel; removing the bronchus, dredging and cleaning; if residual iron sheet remains in the previous experiment, loosening, cleaning and dedusting are needed; uniformly putting the iron sheet with the impurities removed and the rust reduced into the barrel, and uniformly matching the thickness, thinness, excellence and inferiority of the iron sheet;
putting seed crystals, adding clear water, starting a small amount of air, uniformly stirring, and detecting the concentration of the opened barrel;
heating to 75 ℃ within 8 hours, controlling the temperature to be 75-81 ℃ within 24 hours, and controlling the temperature to be 81-89 ℃ after 24 hours; when the concentration is lower in the middle of the reaction, a proper amount of ferrous sulfate, namely seed crystals, is added instantly;
and (3) starting sampling and colorimetric after about 50 hours of reaction, recording the color condition, and carrying out colorimetric 1-2 times every 6-8 hours when the end point is approached, wherein the color is compared with a barreled standard sample: reaching the end point of approximation, micro or slight brightness;
and after the color reaches the end point, immediately closing the air valve, opening the reaction barrel, simultaneously sampling and detecting the barrel release concentration and yield, and completing barrel release within 3 hours.
2. The process for preparing high pigment iron oxide yellow according to claim 1, wherein in the first step, the concentration of the ferrous sulfate solution is controlled to be 35-50g/100ml, and the pH value is controlled to be 4-6.
3. The process for preparing high-pigment iron oxide yellow according to claim 1, wherein in the first step, the concentration of the liquid caustic soda is 30% by mass;
the air inlet amount is 150-200m3Hour/hour; the air volume is 70-90m3In terms of hours.
4. The process for preparing high pigment yellow iron oxide according to claim 1, wherein in the first step, the requirement for detecting the seed crystal is: the pH value is 4-6, the residual iron is 10.00-14.00g/100ml, and the solid content is more than or equal to 3.5g/100 ml.
5. The process for preparing high pigment iron oxide yellow according to claim 1, wherein in the first step, the amount of the air is increased to 150-200m3In terms of hours.
6. The process for preparing high pigment yellow iron oxide according to claim 1, wherein the seed crystal is prepared by the following steps:
1) collecting 3400kg-4500kg ferrous sulfate solution, controlling concentration at 35-50g/100ml, pH value at 4-6, temperature below 37 deg.C, and color light green;
2) measuring 1200kg of liquid caustic soda with the concentration of 30%, and compressing and conveying the liquid caustic soda into a dilute caustic soda tank by using air;
3) cleaning the seed crystal barrel, and checking whether an air pipeline and a bottom valve of the seed crystal barrel are normal;
4) adding 1000ml-5000ml of clear water into the barrel, adding 100ml of sulfuric acid, introducing air and stirring uniformly;
5) adding ferrous sulfate solution, supplementing clear water, and stirring with air for 2 min to make the ferrous sulfate concentration in the barrel about 21g/100ml-23g/100ml and pH value 3-4;
6) the air inlet amount is 150-3Opening a dilution water valve, slowly adding dilute alkali liquor, and controlling the adding within 5-10 minutes;
7) after the alkali is added, the air volume is reduced to 70-90m3Adding dilute alkali solution or adding a small amount of clear water every hour to ensure that the reaction volume is 24m3；
8) Detecting in the reaction process, and stopping the reaction if the seed crystal requirement is met; if the seed crystal is oxidized for 4-9 hours and the gel is formed, the air amount is increased to 150-200m3Hour/hour;
9) oxidizing the seed crystal for 15-25 hours, and then converting the color into earthy yellow to obtain the end point;
10) immediately stopping introducing air for oxidation after the end point is reached, sampling 50ml, and placing the sample in a colorimetric tube for detecting the quality of the seed crystal; the pH value of the seed crystal is required to be 4-6, the residual iron is 10.00-14.00g/100ml, and the solid content is more than or equal to 3.5g/100 ml.
7. The process for preparing high pigment yellow iron oxide according to claim 1, wherein in the second step, the open barrel concentration is 4.0g/100ml-6.0g/100 ml.
8. The process for preparing high pigment yellow iron oxide according to claim 1, wherein in the second step, the amount of air is 70 to 90m until the temperature reaches 75 ℃ within 8 hours3The seed crystal is prevented from being continuously oxidized in one hour; after the temperature is raised to 75 ℃, the air amount is 150-3And (4) turning the air in the barrel uniformly every hour.
9. The process for producing high pigment yellow iron oxide according to claim 1, wherein in the second step, the concentration in the middle of the reaction is controlled to be lower than 4.0g/100ml to 6.0g/100ml at 81 to 89 ℃, and the seed crystal is added immediately.
10. The process for preparing high pigment yellow iron oxide according to claim 1, wherein the process for preparing high pigment yellow iron oxide comprises the following steps:
step one preparation of seed crystals
1) Collecting 3400kg-4500kg ferrous sulfate solution, controlling concentration at 35-50g/100ml, pH value at 4-6, temperature below 37 deg.C, and color light green;
2) measuring 1200kg of liquid caustic soda with the concentration of 30%, and compressing and conveying the liquid caustic soda into a dilute caustic soda tank by using air;
3) cleaning the seed crystal barrel, and checking whether an air pipeline and a bottom valve of the seed crystal barrel are normal;
4) adding 1000ml-5000ml of clear water into the barrel, adding 100ml of sulfuric acid, introducing air and stirring uniformly;
5) adding a ferrous sulfate solution, supplementing clear water, and stirring with air for 2 minutes to ensure that the concentration of the ferrous sulfate in the barrel is about 21-23g/100ml and the pH value is 3-4;
6) the air inlet amount is 150-3Opening a dilution water valve, slowly adding dilute alkali liquor, and controlling the adding within 5-10 minutes;
7) after the alkali is added, the air quantity is reduced to 70-90m3Adding dilute alkali solution or adding a small amount of clear water every hour to ensure that the reaction volume is 24m3；
8) Detecting in the reaction process, and stopping the reaction if the seed crystal requirement is met; if the seed crystal is oxidized for 4-9 hours and the gel is formed, the air amount is increased to 150-200m3Hour/hour;
9) oxidizing the seed crystal for 15-25 hours, and then converting the color into earthy yellow to obtain the end point;
10) immediately stopping introducing air for oxidation after the end point is reached, sampling 50ml, and placing the sample in a colorimetric tube for detecting the quality of the seed crystal; the pH value of the seed crystal is required to be 4-6, the residual iron is 10.00-14.00g/100ml, and the solid content is more than or equal to 3.5g/100 ml;
step two preparation of high-pigment iron oxide yellow
11) Cleaning the oxidation barrel; removing the bronchus, dredging and cleaning; if residual iron sheet remains in the previous experiment, loosening, cleaning and dedusting are needed; uniformly putting the iron sheet with the impurities removed and the rust reduced into the barrel, and uniformly matching the thickness, thinness, excellence and inferiority of the iron sheet;
12) seed crystals are put in and clear water is added for about 12m3Ensure that the volume of the barrel opening reaches 32m3Starting a small amount of air, uniformly stirring, detecting the concentration of the opened barrel, and controlling the concentration to be 4-6g/100 ml;
13) heating to 75 deg.C within 8 hr, and controlling air amount to 70-90m before reaching 75 deg.C3The seed crystal is prevented from being continuously oxidized in one hour; after the temperature is raised to 75 ℃, the air amount is increased to 150-3The air is evenly stirred in the barrel within one hour; the temperature is controlled to be 75-81 ℃ within 24 hours, and after 24 hours, the temperature is controlled to be 81-89 ℃. When the concentration in the middle of the reaction is lower than 4.0-6.0g/100ml, a proper amount of ferrous sulfate is added in emergency;
14) sampling and colorimetric are started after about 50 hours, the color condition is well recorded, the colorimetric is carried out for 1-2 times every 6-8 hours when the end point is approached, and the color is compared with a barreled standard sample: reaching the end point of approximation, micro or slight brightness;
15) and after the color reaches the end point, immediately closing the air valve, opening the reaction barrel, simultaneously sampling and detecting the barrel release concentration and yield, and completing barrel release within 3 hours.
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| CN101225246A (en) * | 2008-01-28 | 2008-07-23 | 升华集团德清华源颜料有限公司 | Special iron oxide yellow pigment for tobacco and production method thereof |
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| CN101225246A (en) * | 2008-01-28 | 2008-07-23 | 升华集团德清华源颜料有限公司 | Special iron oxide yellow pigment for tobacco and production method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 来胜利编著: "《常用精细化工产品研制与生产》", vol. 2006, 陕西科学技术出版社, pages: 119 - 121 * |
| 王之平等: "透明氧化铁黄超微粒子的研制", no. 3, pages 36 - 36 * |
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