CN107033656A - A kind of heat resistant type ferric oxide yellow pigment and preparation method thereof - Google Patents

A kind of heat resistant type ferric oxide yellow pigment and preparation method thereof Download PDF

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Publication number
CN107033656A
CN107033656A CN201710310974.3A CN201710310974A CN107033656A CN 107033656 A CN107033656 A CN 107033656A CN 201710310974 A CN201710310974 A CN 201710310974A CN 107033656 A CN107033656 A CN 107033656A
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oxide yellow
solution
iron oxide
heat resistant
resistant type
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Inventor
潘国祥
李金花
沈辉
徐敏虹
吴周依婷
周佳豪
陆晶晶
郑卫红
倪生良
曹枫
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Huzhou University
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Huzhou University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03Powdery paints
    • C09D5/033Powdery paints characterised by the additives
    • C09D5/038Anticorrosion agents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/02Ingredients treated with inorganic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/22Compounds of iron
    • C09C1/24Oxides of iron
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2272Ferric oxide (Fe2O3)

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

The present invention relates to a kind of heat resistant type ferric oxide yellow pigment and preparation method thereof.Reaction raw materials are used as using soluble alkaline earth salt, calgon and sodium hydroxide, and ultrasonic disperse technology and organic dispersing agent are introduced during cladding, by reacting in ferric oxide yellow pigment Surface coating alkali earth metal phosphate, the composite of formation improves the heat resistance of iron oxide yellow, can be used when plastic processing and powdery paints are applied as colouring agent.The cladded type iron oxide yellow that the present invention is synthesized has heat resistance good, synthetic method is simple, cost is low, safety and environmental protection the advantages of, with higher industrial application value.

Description

A kind of heat resistant type ferric oxide yellow pigment and preparation method thereof
Technical field
The present invention relates to a kind of heat resistant type ferric oxide yellow pigment and preparation method thereof.
Background technology
In recent years, Chinese iron oxide industry comes into the stage of production capacity surplus and competition, and production capacity surplus is whole oxidation The great difficult problem that iron industry faces, the developing ability of ferrous oxide industry of current China is also in the developing stage of extensive style, and product and technique lack Few innovation.Resources advantage can not be changed into economic advantages and technical advantage.
Iron oxide yellow abbreviation iron oxide yellow, is aqueous di-iron trioxide, and molecular formula is FeOOH, and iron oxide yellow is a kind of lemon The yellow powder to brown, due to production method and the difference of operating condition, its crystal structure and physical property have very big difference It is different.The crystallization water can be gradually sloughed when iron oxide yellow is more than 177 DEG C, becomes iron oxide red.Due to iron oxide yellow heat endurance compared with Difference, therefore limited in plastic processing and powdery paints coloring application by larger.
The content of the invention
The present invention is in order to overcome the shortcomings of iron oxide yellow heat resistance, the present invention the in plastic processing and powdery paints application One purpose is a kind of heat resistant type ferric oxide yellow pigment, and second object of the present invention is to provide above-mentioned heat resistant type iron oxide yellow The preparation method of pigment, the present invention is heat-resisting to improve iron oxide yellow in one layer of fine and close alkali earth metal phosphate of iron oxide yellow outer cladding Performance.
Present invention employs following technical scheme:
A kind of heat resistant type ferric oxide yellow pigment, it is characterised in that:The fine and close alkaline-earth metal of iron oxide yellow raw material outer layer covers Phosphate, alkali earth metal phosphate is magnesium, calcium, strontium, the phosphatic one or more of barium, and iron oxide yellow is golden with clad alkaline earth It is 1: 1~100: 1 to belong to phosphatic mass ratio;
The preparation method of described heat resistant type ferric oxide yellow pigment, it is characterised in that this method comprises the following steps:1) Iron oxide yellow is dispersed in water under stirring, iron oxide yellow mixed liquor is formed;2) soluble alkaline earth salt is dissolved in water configuration Into solution A, sodium hydroxide is dissolved in water and is configured to solution B, calgon and is dissolved in water to be configured to solution C;3) then by solution A, Solution B and solution C are added in iron oxide yellow mixed liquor simultaneously under agitation, and carry out ultrasonic disperse, and reaction temperature is controlled 50 ~90 DEG C, continue to stir 0.5~20h after solution is added;Filter cake is dried at 50~105 DEG C after press filtration, washing, powder It is broken, obtain product;
The preparation method of described heat resistant type ferric oxide yellow pigment is characterized in that:Alkali salt is sulfate, nitric acid The one or more of salt or chloride;
The preparation method of described heat resistant type ferric oxide yellow pigment is characterized in that:Alkali salt, calgon, hydrogen The mol ratio of sodium oxide molybdena is 1: 1: 1~1.3;
The preparation method of described heat resistant type ferric oxide yellow pigment is characterized in that:Step 1) in be additionally added polyethylene glycol, Lauryl sodium sulfate, the one or more of neopelex.
The composite that the present invention is formed by alkali earth metal phosphate coated iron oxide Huang improves the resistance to of iron oxide yellow It is hot, it can be used when plastic processing and powdery paints are applied as colouring agent.The cladded type iron oxide yellow that the present invention is synthesized by In introducing ultrasonic disperse technology and organic dispersing agent during cladding so that alkali earth metal phosphate clad is more complete, Product has heat resistance good, synthetic method is simple, cost is low, safety and environmental protection the advantages of, with higher industrial application value.
Embodiment
This specific embodiment be only explanation of the invention its be not limitation of the present invention, those skilled in the art This example can be made as needed after this specification is read without innovative modification, but as long as wanting in the present invention All protected in the range of asking by Patent Law.
Embodiment 1
20Kg ferric oxide yellow pigment 810# are weighed, iron oxide yellow is dispersed in 200L water under stirring, oxidation is formed Iron oxide yellow content is 10% mixed liquor;2.4Kg magnesium sulfate, 0.8Kg sodium hydroxides, 2.04Kg calgons are weighed respectively, point 100L water is not dissolved in is configured to solution A, solution B and solution C;Then solution A, solution B and solution C are added simultaneously under agitation In iron oxide yellow mixed liquor, and ultrasonic disperse is carried out, reaction temperature is controlled at 80 DEG C, continue to stir 3h after solution is added;Through Filter cake is dried at 90 DEG C after press filtration, washing, crushed, heat resistant type iron oxide yellow product A is obtained.
Embodiment 2
10Kg ferric oxide yellow pigment 810# are weighed, iron oxide yellow is dispersed in 200L water under stirring, oxidation is formed Iron oxide yellow content is 5% mixed liquor;9.84Kg calcium nitrate, 2.4Kg sodium hydroxides, 6.12Kg calgons are weighed respectively, point 30L water is not dissolved in is configured to solution A, solution B and solution C;Then solution A, solution B and solution C are added simultaneously under agitation In iron oxide yellow mixed liquor, and ultrasonic disperse is carried out, reaction temperature is controlled at 70 DEG C, continue to stir 10h after solution is added;Through Filter cake is dried at 100 DEG C after press filtration, washing, crushed, heat resistant type iron oxide yellow product B is obtained.
Embodiment 3
30Kg ferric oxide yellow pigment 810# are weighed, iron oxide yellow is dispersed in 100L water under stirring, oxidation is formed Iron oxide yellow content is 30% mixed liquor;3.16Kg strontium chlorides, 0.88Kg sodium hydroxides, 2.04Kg calgons are weighed respectively, 80L water is dissolved in respectively is configured to solution A, solution B and solution C;Then solution A, solution B and solution C are added simultaneously under agitation Enter in iron oxide yellow mixed liquor, and carry out ultrasonic disperse, reaction temperature is controlled at 50 DEG C, continue to stir 18h after solution is added; Filter cake is dried at 80 DEG C after press filtration, washing, crushed, heat resistant type iron oxide yellow product C is obtained.
Embodiment 4
30Kg ferric oxide yellow pigment 810# are weighed, iron oxide yellow is dispersed in 100L water under stirring, oxidation is formed Iron oxide yellow content is 30% mixed liquor;4.16Kg barium chlorides, 0.88Kg sodium hydroxides, 2.04Kg calgons are weighed respectively, 80L water is dissolved in respectively is configured to solution A, solution B and solution C;Then solution A, solution B and solution C are added simultaneously under agitation Enter in iron oxide yellow mixed liquor, and carry out ultrasonic disperse, reaction temperature is controlled at 70 DEG C, continue to stir 18h after solution is added; Filter cake is dried at 80 DEG C after press filtration, washing, crushed, heat resistant type iron oxide yellow product D is obtained.
Heat resistance is tested:Product 2.5g is weighed, is fitted into small crucible in 260 DEG C of baking ovens and heats 0.5h, is cooled down after taking-up, Then the value of chromatism Δ E before and after test product is toasted on spectrophotometric color measurement instrument.Obtain heat resistant type iron oxide yellow product A, heat resistant type Iron oxide yellow product B, heat resistant type iron oxide yellow product C, heat resistant type iron oxide yellow product D Δ E are respectively 2.46,1.73, 2.08,3.28.
Embodiment 5
20Kg ferric oxide yellow pigment 810# and 0.05Kg polyethylene glycol is weighed, it is under stirring that iron oxide yellow and polyethylene glycol is equal It is even to be scattered in 200L water, form the mixed liquor that iron oxide yellow content is 10%;2.4Kg magnesium sulfate, 0.8Kg hydrogen-oxygens are weighed respectively Change sodium, 2.04Kg calgons, 100L water is dissolved in respectively and is configured to solution A, solution B and solution C;Then by solution A, solution B and solution C are added in iron oxide yellow mixed liquor simultaneously under agitation, and carry out ultrasonic disperse, and reaction temperature is controlled at 80 DEG C, treated Solution continues to stir 3h after adding;Filter cake is dried at 90 DEG C after press filtration, washing, crushed, heat resistant type iron oxide yellow is obtained Product E.
Embodiment 6
10Kg ferric oxide yellow pigment 810# and 0.08Kg lauryl sodium sulfate is weighed, by iron oxide yellow and 12 under stirring Sodium alkyl sulfate is dispersed in 200L water, forms the mixed liquor that iron oxide yellow content is 5%;9.84Kg nitric acid is weighed respectively Calcium, 2.4Kg sodium hydroxides, 6.12Kg calgons, are dissolved in 30L water and are configured to solution A, solution B and solution C respectively;Then Solution A, solution B and solution C are added in iron oxide yellow mixed liquor simultaneously under agitation, and carry out ultrasonic disperse, reaction temperature Control continues to stir 10h at 70 DEG C after solution is added;Filter cake is dried at 100 DEG C after press filtration, washing, crushed, is obtained Heat resistant type iron oxide yellow product F.
Embodiment 7
30Kg ferric oxide yellow pigment 810# and 0.1Kg polyethylene glycol is weighed, it is under stirring that iron oxide yellow and polyethylene glycol is equal It is even to be scattered in 100L water, form the mixed liquor that iron oxide yellow content is 30%;3.16Kg strontium chlorides, 0.88Kg hydrogen are weighed respectively Sodium oxide molybdena, 2.04Kg calgons, are dissolved in 80L water and are configured to solution A, solution B and solution C respectively;Then by solution A, molten Liquid B and solution C are added in iron oxide yellow mixed liquor simultaneously under agitation, and carry out ultrasonic disperse, and reaction temperature is controlled at 50 DEG C, Continue to stir 18h after solution is added;Filter cake is dried at 80 DEG C after press filtration, washing, crushed, heat resistant type iron oxide is obtained Yellow product G.
Embodiment 8
30Kg ferric oxide yellow pigment 810# and 0.1Kg neopelexes are weighed, by iron oxide yellow and ten under stirring Dialkyl benzene sulfonic acids sodium is dispersed in 100L water, forms the mixed liquor that iron oxide yellow content is 30%;Weigh respectively 4.16Kg barium chlorides, 0.88Kg sodium hydroxides, 2.04Kg calgons, be dissolved in respectively 80L water be configured to solution A, solution B and Solution C;Then solution A, solution B and solution C are added in iron oxide yellow mixed liquor simultaneously under agitation, and carries out ultrasound point Dissipate, reaction temperature is controlled at 70 DEG C, continue to stir 18h after solution is added;Filter cake is dried at 80 DEG C after press filtration, washing Dry, crushing, obtains heat resistant type iron oxide yellow product H.
Heat resistance is tested:Product 2.5g is weighed, is fitted into small crucible in 260 DEG C of baking ovens and heats 0.5h, is cooled down after taking-up, Then the value of chromatism Δ E before and after test product is toasted on spectrophotometric color measurement instrument.Obtain heat resistant type iron oxide yellow product E, heat resistant type Iron oxide yellow product F, heat resistant type iron oxide yellow product G, heat resistant type iron oxide yellow product H Δ E are respectively 2.06,1.33, 1.85,2.48.
Test indicate that, ultrasonic disperse technology and organic dispersing agent, the alkaline-earth metal phosphorus of synthesis are introduced during cladding Hydrochlorate coated iron oxide Huang product has excellent heat resistance, can be used as plastic processing and powdery paints colouring agent at 260 degree Use.

Claims (5)

1. a kind of heat resistant type ferric oxide yellow pigment, it is characterised in that:The fine and close alkaline-earth metal phosphorus of ferric oxide yellow pigment outer layer covers Hydrochlorate, alkali earth metal phosphate is magnesium, calcium, strontium, the phosphatic one or more of barium, iron oxide yellow and clad alkaline-earth metal Phosphatic mass ratio is 1: 1~100: 1.
2. a kind of method of the heat resistant type ferric oxide yellow pigment prepared described in claim 1, it is characterised in that this method include with Under step:
1) iron oxide yellow is dispersed in water under stirring, iron oxide yellow mixed liquor is formed;
2) soluble alkaline earth salt is dissolved in water and is configured to solution A, sodium hydroxide is dissolved in water and is configured to solution B, hexa metaphosphoric acid Sodium is dissolved in water and is configured to solution C;
3) and then by solution A, solution B and solution C add simultaneously in iron oxide yellow mixed liquor under agitation, and carry out ultrasound point Dissipate, reaction temperature is controlled at 50~90 DEG C, continue to stir 0.5~20h after solution is added;Filter cake is existed after press filtration, washing Dry, crush at 50~105 DEG C, obtain product.
3. the preparation method of heat resistant type ferric oxide yellow pigment according to claim 2 is characterized in that:Alkali salt is The one or more of sulfate, nitrate or chloride.
4. the preparation method of heat resistant type ferric oxide yellow pigment according to claim 2 is characterized in that:Alkali salt, six Sodium metaphosphate, the mol ratio of sodium hydroxide are 1: 1: 1~1.3.
5. the preparation method of heat resistant type ferric oxide yellow pigment according to claim 2 is characterized in that:Step 1) in also plus Enter the one or more of polyethylene glycol, lauryl sodium sulfate, neopelex.
CN201710310974.3A 2017-05-02 2017-05-02 A kind of heat resistant type ferric oxide yellow pigment and preparation method thereof Pending CN107033656A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112980220A (en) * 2020-11-25 2021-06-18 正太新材料科技有限责任公司 Preparation method and application of low-oil-absorption high-temperature-resistant iron oxide coating
CN113388268A (en) * 2021-06-18 2021-09-14 浙江华源颜料股份有限公司 Iron oxide black pigment with near-infrared reflection function and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4082905A (en) * 1976-06-04 1978-04-04 Bayer Aktiengesellschaft Production of iron oxide pigments with improved resistance to oxidation

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4082905A (en) * 1976-06-04 1978-04-04 Bayer Aktiengesellschaft Production of iron oxide pigments with improved resistance to oxidation

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈健: "包覆型氧化铁系颜料微结构与耐热性能研究", 《中国学位论文全文数据库》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112980220A (en) * 2020-11-25 2021-06-18 正太新材料科技有限责任公司 Preparation method and application of low-oil-absorption high-temperature-resistant iron oxide coating
CN113388268A (en) * 2021-06-18 2021-09-14 浙江华源颜料股份有限公司 Iron oxide black pigment with near-infrared reflection function and preparation method thereof

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Application publication date: 20170811