CN101225246B - Special iron oxide yellow pigment for tobacco and production method thereof - Google Patents
Special iron oxide yellow pigment for tobacco and production method thereof Download PDFInfo
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- CN101225246B CN101225246B CN2008100596118A CN200810059611A CN101225246B CN 101225246 B CN101225246 B CN 101225246B CN 2008100596118 A CN2008100596118 A CN 2008100596118A CN 200810059611 A CN200810059611 A CN 200810059611A CN 101225246 B CN101225246 B CN 101225246B
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Abstract
The invention relates to an iron oxide yellow pigment for tobacco and the production method, which resolves the technical problem and aims at providing a new liquid-liquid reacting iron oxide yellow pigment and the production method for tobacco, thus can ensure that the granularity of the product is more refined, more symmetrical and brighter than that made by iron filing method. The iron oxide yellow pigment for tobacco also aims at controlling the content of arsenic and lead in product in order to reach the requirement of tobacco industry. The production method adopts the technical proposal that the iron oxide yellow pigment is obtained by the reaction of 4500 to 5000 weight parts of solid green copperas with 80 to 88 percent content and 2500 to 300 weight parts of sodium hydroxide solution with 32 percent concentration. The production method comprises the inoculating seed preparation and the second oxidation. The an iron oxide yellow pigment can be widely used in tobacco industry, such as tipping paper makers and printing ink makers.
Description
Technical field
The present invention relates to a production method that grows tobacco special-purpose ferric oxide yellow pigment.Can be widely used in tobacco industry, as producers such as yew paper, printing ink.
Background technology
The special-purpose ferric oxide yellow pigment of tobacco, its chemical name: ferric oxide or hydrous iron oxide, chemical molecular formula: Fe
2O
3H
2O (or FeOOH) is the important source material of producing yew paper, printing ink.Producing the special-purpose ferric oxide yellow pigment of tobacco at present generally adopts the iron sheet method to produce, in whole process of production, there is iron sheet to participate in reaction, this Nonrenewable resources of iron have not only been consumed, and the product of producing is no matter on fineness, still all not ideal enough on the product performance, can not be effectively controlled as the content of poisonous heavy metal arsenic (As) and lead (Pb).In addition, on production technique, there is phenomenon dirty, random, difference unavoidably.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of brand-new, belong to the production method of the special-purpose ferric oxide yellow pigment of tobacco of liquid-liquid phase reaction, make the granularity of the product that obtains than the exquisiteness of iron sheet method, even, bright-colored; Another purpose is arsenic and a plumbous content in the control product, to reach the requirement that tobacco industry uses.In addition, whole technological process does not have iron sheet to participate in reaction, to scheme to save iron resources; The level of automation of improve producing changes and produces the phenomenon that goes up dirty, unrest, difference at present.
The technical solution adopted in the present invention is: the production method of the special-purpose ferric oxide yellow pigment of tobacco comprises crystal seed preparation and second oxidation, and production stage is as follows:
I) crystal seed prepares part,
A) with content be 80～88% ferrous being dissolved in water of solid sulphuric acid, clarification claims that content is that 40% clarification copperas solution 1700～2500 weight parts drop in the crystal seed reaction container;
B) be that 32% sodium hydroxide solution 200～280 weight parts drop in the crystal seed reaction container with concentration;
C) at normal temperatures, make ferrous sulfate and sodium hydroxide carry out neutralization reaction, the bubbling air oxidation, oxidization time is 12～18 hours, and final ferrous hydroxide is oxidized to the iron oxide yellow crystal seed, and surplus ferrous sulfate content keeps 10～30% weight parts;
Ii) second oxidation part,
D) crystal seed of making is dropped in the reaction container, add a certain amount of water latting drown then, control ferrous sulfate content 5～15% weight parts, ferrous sulfate content is more than 5% in the maintenance reaction container in entire reaction course, when being lower than this content, in time add ferrous sulfate;
E) open the steam valve heating, after temperature reaches 60 ℃, open stirrer and blast air, control air quantity 150～400m
3/ h:
F) the liquid caustic soda continuously and smoothly of latting drown 5～15% concentration be added dropwise in the reaction container, pH value controls to 2.5～3.5, rate of addition is decided on the response situation of feed liquid in pH value and the bucket, temperature in the entire reaction course is controlled between 60～88 ℃, when being reacted to 20～35 hours, observe in the bucket feed liquid color and standard near the time, begin to scrape sample and detect, and the interior ferrous sulfate content of control bucket, until color and standard specimen little like the time, stop liquid caustic soda and drip, the steam off valve still stirs and blasts air, sample is approximate to color and standard specimen, stop to stir, turn off air door, prepare to put bucket.
The invention has the beneficial effects as follows: 1) the present invention adopts brand-new pure liquid phase production technology production, in process of production starting material are carried out strict screening, get rid of the higher raw material of heavy metal content, just heavy metal content is effectively controlled in the making source, two important indicators are arsenic (As)≤10mg/kg and lead (Pb)≤20mg/kg, conventional index is controlled according to the scope of common ferric oxide national Specification in addition, all within country-level product control; 2) in the whole production reaction process, do not have iron sheet to participate in reaction, not only saved iron resources, and the granularity of the product that obtains than the exquisiteness of iron sheet method, evenly, purity is high; 3) product has good color opacifying power, tinting strength, heat-resisting, anti-solvent, advantage such as nontoxic, and purer than common iron oxide pigment, and color is more bright-coloured; 4) this production technique can change phenomenon dirty in the present production, random, difference fully, improves the automatic production degree.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
The present invention's liquid phase production technology is to be carrier with the crystal seed, under hot state, adopt ferrous sulfate and sodium hydroxide under acidic conditions, in the oxidation bucket, react, generate ferrous hydroxide, bubbling air is that oxygenant carries out oxidizing reaction with oxygen, form iron oxide yellow, its reaction formula is as follows:
FeSO
4+2NaOH＝＝Fe(OH)
2+Na
2SO
4
Embodiment one, and as shown in Figure 1, this routine ferric oxide yellow pigment is that ferrous to be dissolved in water, to clarify back and concentration be that 32% sodium hydroxide solution reaction forms for 80～88% solid sulphuric acid by content.
The production method of described ferric oxide yellow pigment comprises crystal seed preparation and second oxidation, and processing step is as follows:
I) crystal seed preparation,
A) being that 81.6% solid sulphuric acid is ferrous with content is dissolved in water, clarifies, and claims that content is that about 39.6% copperas solution 1894kg (amount to content 100% and be 750kg) drops in the crystal seed reaction container;
B) be that 32% sodium hydroxide solution 210kg joins in the crystal seed reaction container with concentration;
C) at normal temperatures, make ferrous sulfate and sodium hydroxide carry out neutralization reaction, the bubbling air oxidation, oxidization time is 12.4 hours, final ferrous hydroxide is oxidized to iron oxide yellow crystal seed (Fe
2O
3H
2O), surplus ferrous sulfate content keeps 12.8%;
Ii) second oxidation,
D) crystal seed of making is dropped in the reaction container, add a certain amount of water latting drown then, control ferrous sulfate content 6.95%, ferrous sulfate content is more than 5% in the maintenance reaction container in entire reaction course, when being lower than this content, in time add ferrous sulfate;
E) open the steam valve heating, when temperature reaches 60 ℃, open stirrer and blast air, control air quantity 150m
3/ h;
F) the liquid caustic soda continuously and smoothly of latting drown 5% concentration be added dropwise in the reaction container, pH value controls to 2.5～3.5, rate of addition is decided on the response situation of feed liquid in pH value and the bucket, and temperature of reaction slowly raise along with the time, and air quantity also is to strengthen gradually along with the reaction times.Temperature in the entire reaction course is controlled between 60～88 ℃, and temperature control divides a three phases, and 1, reaction (about 0～8 hour) temperature in early stage is controlled at 60～70 ℃; 2, reaction (about 8～20 hours) temperature in mid-term is controlled to be 71～80 ℃; 3, reaction later stage (more than 20 hours) temperature is controlled to be 81～88 ℃; Temperature-rise period is wanted slowly steadily.Be reacted to 23 hours, feed liquid color and standard are approaching in the bucket, begin to scrape sample, and ferrous sulfate content in the control bucket, until color and standard specimen little like the time, stop dropwise liquid, the steam off valve still stirs and blasts air, sample is approximate to color and standard specimen, stop to stir, turn off air door, prepare to put bucket.
Embodiment two, and as shown in Figure 1, this routine ferric oxide yellow pigment is that ferrous to be dissolved in water, to clarify back and concentration be that 32% sodium hydroxide solution reaction forms for 88% solid sulphuric acid by content.
The production method of described ferric oxide yellow pigment comprises crystal seed preparation and second oxidation, and processing step is as follows:
I) crystal seed preparation,
A) being that 87.6% solid sulphuric acid is ferrous with content is dissolved in water, clarifies, and claims that content is that about 41.0% copperas solution 2440kg (amount to content 100% and be 100kg) drops in the crystal seed reaction container;
B) be that 32% sodium hydroxide solution 280kg adds in the crystal seed reaction container with concentration;
C) at normal temperatures, make ferrous sulfate and sodium hydroxide carry out neutralization reaction, the bubbling air oxidation, oxidization time is 16.5 hours, final ferrous hydroxide is oxidized to iron oxide yellow crystal seed (Fe
2O
3H
2O), surplus ferrous sulfate content keeps 25.4% weight part;
Ii) second oxidation,
D) crystal seed of making is dropped in the reaction container, add a certain amount of water latting drown then, control ferrous sulfate content 12.51% weight part; Ferrous sulfate content is more than 5% in the maintenance oxidation bucket in entire reaction course, when being lower than this content, in time add ferrous sulfate;
E) open the steam valve heating, temperature reaches 63 ℃, opens stirrer and blasts air, control air quantity 200m
3/ h;
F) the liquid caustic soda continuously and smoothly of latting drown 13.6% concentration be added dropwise in the reaction container, pH value controls to 2.5～3.5, rate of addition is decided on the response situation of feed liquid in pH value and the bucket, and temperature of reaction slowly raise along with the time, and air quantity also is to strengthen gradually along with the reaction times.Temperature in the entire reaction course is controlled between 60～88 ℃, and temperature control divides a three phases, and 1, reaction (about 0～8 hour) temperature in early stage is controlled at 60～70 ℃; 2, reaction (about 8～20 hours) temperature in mid-term is controlled to be 71～80 ℃; 3, reaction later stage (more than 20 hours) temperature is controlled to be 81～88 ℃; Temperature-rise period is wanted slowly steadily.When being reacted to 30 hours, see barrel interior feed liquid color and standard near the time, begin to scrape sample, and a ferrous content in the control bucket, until color and standard specimen little like the time, stop dropwise liquid, the steam off valve still stirs and blasts air, sample is approximate to color and standard specimen, stop to stir, turn off air door, prepare to put bucket.
Embodiment three, and as shown in Figure 1, this routine ferric oxide yellow pigment is that ferrous to be dissolved in water, to clarify back and concentration be that 32% sodium hydroxide solution reaction forms for 86% solid sulphuric acid by content.
The production method of described ferric oxide yellow pigment comprises crystal seed preparation and second oxidation, and processing step is as follows:
I) crystal seed preparation,
A) being that 86.3% solid sulphuric acid is ferrous with content is dissolved in water, clarifies, and claims that content is that about 38.6% copperas solution 2200kg (amount to content 100% and be 850kg) drops in the crystal seed reaction container;
B) be that 32% sodium hydroxide solution 240kg drops in the crystal seed reaction container with concentration;
C) at normal temperatures, make ferrous sulfate and sodium hydroxide carry out neutralization reaction, the bubbling air oxidation, oxidization time is 14 hours, final ferrous hydroxide is oxidized to iron oxide yellow crystal seed (Fe
2O
3H
2O), surplus ferrous sulfate content keeps 18.1% weight part;
Ii) second oxidation,
D) crystal seed of making is dropped in the reaction container, add a certain amount of water latting drown then, control ferrous sulfate content 9.31% weight part,
E) open the steam valve heating, temperature reaches 65 ℃, opens stirrer and blasts air, control air quantity 150m
3/ h;
F) the liquid caustic soda continuously and smoothly of latting drown 9% concentration be added dropwise in the reaction container, pH value controls to 2.5～3.5, rate of addition is decided on the response situation of feed liquid in pH value and the bucket, and temperature of reaction slowly raise along with the time, and air quantity also is to strengthen gradually along with the reaction times.Temperature in the entire reaction course is controlled between 60～88 ℃, and temperature control divides a three phases, and 1, reaction (about 0～8 hour) temperature in early stage is controlled at 60～70 ℃; 2, reaction (about 8～20 hours) temperature in mid-term is controlled to be 71～80 ℃; 3, reaction later stage (more than 20 hours) temperature is controlled to be 81～88 ℃; Temperature-rise period is wanted slowly steadily.When being reacted to 28 hours, see barrel interior feed liquid color and standard near the time, begin to scrape sample, and a ferrous content in the control bucket, until color and standard specimen little like the time, stop dropwise liquid, the steam off valve still stirs and blasts air, sample is approximate to color and standard specimen, stop to stir, turn off air door, prepare to put bucket.
In the reaction of the various embodiments described above, copperas solution and sodium hydroxide solution all add in each step respectively as requested, the liquefaction of solid sulphuric acid ferrous can be carried out in batches, also can primary treatment, and concentration be 32% sodium hydroxide solution is outsourcing, and the concentration when buying just prepares.When reaction finished in each embodiment, the ferrous sulfate content control in the oxidation bucket was low more good more, and perfect condition is ferrous sulfate and sodium hydroxide complete reaction, residue content is zero, but in order to improve speed of reaction, ferrous sulfate must have residue, general final being controlled at below 3.0.
Intermediate controlled among Fig. 1 refers to step d) among the embodiment, e), f) related control; Back road is handled and referred to: wet feed sieves, filters rinsing, drying, pulverizing, inspection after construction.
Claims (1)
1. a production method that grows tobacco special-purpose ferric oxide yellow pigment is characterized in that this method comprises crystal seed preparation and second oxidation, and production stage is as follows:
I) crystal seed prepares part,
A) with content be 80～88% ferrous being dissolved in water of solid sulphuric acid, clarification claims that content is that 40% clarification copperas solution 1700～2500 weight parts drop in the crystal seed reaction container;
B) be that 32% sodium hydroxide solution 200～280 weight parts drop in the crystal seed reaction container with concentration;
C) at normal temperatures, make ferrous sulfate and sodium hydroxide carry out neutralization reaction, the bubbling air oxidation, oxidization time is 12～18 hours, and final ferrous hydroxide is oxidized to the iron oxide yellow crystal seed, and surplus ferrous sulfate content keeps 10～30% weight parts;
Ii) second oxidation part,
D) crystal seed of making is dropped in the reaction container, add a certain amount of water latting drown then, control ferrous sulfate content 5～15% weight parts, ferrous sulfate content is more than 5% in the maintenance reaction container in entire reaction course, when being lower than this content, in time add ferrous sulfate;
E) open the steam valve heating, after temperature reaches 60 ℃, open stirrer and blast air, control air quantity 150～400m
3/ h;
F) the liquid caustic soda continuously and smoothly of latting drown 5～15% concentration be added dropwise in the reaction container, the pH value controls to 2.5～3.5, rate of addition is decided on the response situation of feed liquid in pH value and the bucket, temperature in the entire reaction course is controlled between 60～88 ℃, when being reacted to 20～35 hours, observe in the bucket feed liquid color and standard near the time, begin to scrape sample and detect, and the interior ferrous sulfate content of control bucket, until color and standard specimen little like the time, stop liquid caustic soda and drip, the steam off valve still stirs and blasts air, sample is approximate to color and standard specimen, stop to stir, turn off air door, prepare to put bucket.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102616862A (en) * | 2012-02-21 | 2012-08-01 | 升华集团德清华源颜料有限公司 | Method for preparing nano-sized transparent yellow iron oxide pigments |
| CN102604435A (en) * | 2012-02-21 | 2012-07-25 | 升华集团德清华源颜料有限公司 | Nano transparent iron oxide yellow pigment |
| CN102603010A (en) * | 2012-02-21 | 2012-07-25 | 升华集团德清华源颜料有限公司 | Transparent nanometer iron oxide red pigment |
| CN106219611B (en) * | 2016-07-27 | 2017-07-11 | 升华集团德清华源颜料有限公司 | A kind of low viscosity iron oxide yellow |
| CN111960475A (en) * | 2020-08-26 | 2020-11-20 | 湖南三环颜料有限公司 | Preparation process of high-pigment iron oxide yellow |
| CN113104901B (en) * | 2021-04-13 | 2024-02-09 | 江西理工大学 | Method for preparing iron oxide yellow from rare earth waste acid leaching slag |
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| CN1415666A (en) * | 2002-12-04 | 2003-05-07 | 中国化工建设总公司常州涂料化工研究院 | Method for producing the yellow pigment of ferric oxide from ferrous sulphate of byproduct abolished by titanium white |
| CN1766005A (en) * | 2005-08-23 | 2006-05-03 | 奚长生 | Method for preparing high purity iron oxide yellow and iron oxide red using titanium dioxide byproduct ferrous sulfate |
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2008
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Patent Citations (3)
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| CN1143611A (en) * | 1995-08-24 | 1997-02-26 | 廖维炎 | Method for producing iron oxide yellow using sulfuric acid roasting residue |
| CN1415666A (en) * | 2002-12-04 | 2003-05-07 | 中国化工建设总公司常州涂料化工研究院 | Method for producing the yellow pigment of ferric oxide from ferrous sulphate of byproduct abolished by titanium white |
| CN1766005A (en) * | 2005-08-23 | 2006-05-03 | 奚长生 | Method for preparing high purity iron oxide yellow and iron oxide red using titanium dioxide byproduct ferrous sulfate |
Non-Patent Citations (3)
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Address after: 313200, Zhejiang, Deqing County province bell town landscape crossing Patentee after: Zhejiang Huayuan pigment Limited by Share Ltd Address before: 313220, Zhejiang, Deqing County province bell town landscape crossing Patentee before: Shenghua Group Deqing Huayuan Pigment Co., Ltd. |