CN101275038B - Special dispersant compound for iron phthalein green and preparation thereof - Google Patents
Special dispersant compound for iron phthalein green and preparation thereof Download PDFInfo
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- CN101275038B CN101275038B CN2007100384730A CN200710038473A CN101275038B CN 101275038 B CN101275038 B CN 101275038B CN 2007100384730 A CN2007100384730 A CN 2007100384730A CN 200710038473 A CN200710038473 A CN 200710038473A CN 101275038 B CN101275038 B CN 101275038B
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Abstract
The invention relates to a dispersant composition exclusively for iron phthalocyanine green, and according to weight consists of 10 to 20 percent of unsaturated fatty acid, two unsaturated fatty acid ester respectively with 1 to 5 percent, 1 to 5 percent of unsaturated amide, 1 to 5 percent of functional monomer, 10 to 15 percent of alkylphenol polypolyoxyethylene ether, 0.1 to 1 percent of initiator, and 20 to 40 percent of liquid alkine with the concentration of 30 percent, and the remained is deioned water. The preparation process of the dispersant composition comprises: 1) the preparation process of mixed monomer; 2) preparing initiator liquid; 3) the preparation process of the dispersant composition through polymerization. The water solution of iron phthalocyanine green dye prepared from the invention can pass Europe standard, thus possessing broad market prospect.
Description
Technical field
The present invention relates to the pigment industry in the chemical industry field, i.e. a kind of special assistant of specific pigment specifically, relates to a kind of cement, mixes earth, mortar goods veridian---special dispersant compound that the iron phthalein is green and preparation method thereof.
Background technology
The iron phthalein is green to add that with its exclusive fast light, weather-proof, alkaline-resisting, corrosion-resistant, high performance such as painted it is cheap, has become the veridian of the painted first-selection of cement, is widely used in concrete and the mortar product.The green year output of domestic iron phthalein is above 10,000 tons.As everyone knows, the iron phthalein is green to be a kind of composite pigment, formulated by a certain percentage by iron oxide yellow and two kinds of pigment of phthalocyanine blue, but phthalocyanine blue is a pigment dyestuff, have very strong hydrophobicity, its energy and the very strong iron oxide yellow of wetting ability are balancedly pieced together mixed together, at first will carry out modification its surface, make it become wetting ability from hydrophobicity, this carries out coating with regard to a kind of aqueous dispersant of needs to it and handles.
The production method that the conventional iron phthalein is green is that phthalocyanine blue is added 5881D, soak more than 24 hours, add ferric oxide bloom and water and be mixed with the slurry of 50% solid content, send into high speed dispersor and carry out high-speed stirring, after slurry reaches uniform degree, after stack gas fluidisation drying, pulverize, piece together and mix, pack.The main component of described 5881D is a sodium dibutyl naphthalene sulfonate, and it is cheap, and is also good as the surface treatment agent effect of phthalocyanine blue, but maximum shortcoming is exactly to need the amount of interpolation very big, and general addition is 2.6-2.8 times of phthalocyanine blue powder.The iron phthalein of producing with 5881D is green to have run into the problem that the pigment water solubles exceeds standard to state's outer vent the time, substitute 5881D and handle phthalocyanine blue so a kind of new dispersion agent is badly in need of in pigment factory.The dispersion agent that is exclusively used in phthalocyanine blue both at home and abroad is quite a few, but the problem that the ubiquity consumption is big, price is expensive, being used to make aqueous color paste can bear, and just seems too high but be used to make its cost of pigment.
Summary of the invention
At the problems referred to above, the present invention aims to provide special dispersant compound of a kind of iron phthalein phthalocyanine and preparation method thereof, can play tangible modifying function to the phthalocyanine blue pigment surface by the present invention, its cost is close with the cost that uses 5881D, technical indicator also can meet the demands, especially the water solubles index that the iron phthalein that makes is green can be passed through European standard, thereby has vast market prospect.That is to say, purpose of the present invention is exactly to adapt to the requirement of European standard to the green water solubles of iron phthalein, utilize unsaturated fatty acids, unsaturated fatty acid ester, unsaturated amides to be main raw material, under the initiator effect, carry out double-bond polymerization, produce the suitable macromolecular compound of the polymerization degree, with the alkali lye neutralization, generate the narrower dispersant with high efficiency of molecular weight ranges subsequently.It is compared with other pigment dyestuff dispersion agent, and it is few to have a consumption, dispersion efficiency height, advantage such as the water solubles is few after the colo(u)rant dispersion, and cost is suitable.
The present invention is achieved in that it is a kind of special dispersant compound for iron phthalein green, it is characterized in that in weight percent the composition of said composition comprises:
Unsaturated fatty acids 10～20
Unsaturated fatty acid ester A 1～5
Unsaturated fatty acid ester B 1～5
Unsaturated amides 1～5
Functional monomer 1～5
Initiator 0.1～1
Liquid caustic soda 20～40
Alkylphenol polyoxyethylene 10～15, last, add to 100 weight % with deionized water.In above-mentioned composition, if the proportioning of each main component changes into, in weight percent, unsaturated fatty acids 14～16%, unsaturated fatty acid ester A3～5%, unsaturated fatty acid ester B4～5%, unsaturated amides 3～5%, functional monomer 1～2%, initiator 0.5～1%, better effects if.
Unsaturated fatty acids described in the above-mentioned composition is selected from a kind of in vinylformic acid, 2-butylene acid, 3-butenoic acid, the acid of 3-methyl-2-butene, the 2-methyl-2-pentenoic acid.
Described unsaturated fatty acid ester A is selected from a kind of in butyl acrylate, 2-butylene acid butyl ester, 3-butyl crotonate, 3-methyl-2-butene acid butyl ester, the 2-methyl-2-pentenoic acid butyl ester.
Described unsaturated fatty acid ester B is selected from Isooctyl acrylate monomer, the different monooctyl ester of 2-butylene acid, the different monooctyl ester of 3-butenoic acid, the different monooctyl ester of 3-methyl-2-butene acid, the 2-methyl-different monooctyl ester of 2-pentenoic acid and chooses any one kind of them.
Described unsaturated amides is selected from a kind of in acrylamide, N hydroxymethyl acrylamide, N,N-DMAA, the N-N-isopropylacrylamide.
Described functional monomer is selected from a kind of in ethoxylation propylene or the ethyl vinyl ether.
Described initiator is selected from a kind of in Ammonium Persulfate 98.5, dibenzoyl peroxide, tert-butyl peroxide hydrogen, the Diisopropyl azodicarboxylate.
Described alkylphenol polyoxyethylene is selected from a kind of in polyoxyethylene octylphenol ether, the polyoxyethylene nonylphenol ether.
According to the present invention, the preparation process of described special dispersant compound for iron phthalein green comprises the following steps:
(1) by after the proportioning weighing unsaturated fatty acids, unsaturated fatty acid ester A, unsaturated fatty acid ester B, unsaturated amides, functional monomer being placed container, stirring and dissolving is even, and it is stand-by to obtain mix monomer;
(2) initiator is added in appropriate amount of deionized water or the monomer stand-by after the stirring and dissolving;
(3) in the reaction vessel that condenser, electric mixer, thermometer, dropping funnel are housed, add proper amount of deionized water, heat up and stir, when temperature rises to 82 ℃, beginning drips above-mentioned ready initiator and mix monomer simultaneously, keep temperature of reaction at 86～90 ℃, 4～6h drips off, drip off back insulation 0.5～1.5h, slowly add liquid caustic soda then, add and stir 15～25min, the alkylphenol polyoxyethylene that adds formula ratio stirs, and 100 orders filter discharging and obtain described disperser composition.
A kind of good dispersant needs certain polymerization degree, and its molecular weight is limited within the narrow scope.The low wettability effect that helps to obtain pigment particles of the polymerization degree, but its molecular weight is too small, can cause dispersion effect poor, and the unit addition also can correspondingly increase; And the polymerization degree is too high, and dispersion agent itself water-soluble bad is poor to the wettability effect of pigment particles, forms " bridging " during dispersion easily, produces flocculation.The green dispersant special of iron phthalein according to the present invention's preparation has the comparatively ideal polymerization degree, so the dispersion effect of granules of pigments is splendid, the green product performance of iron phthalein that make are also more satisfactory, the addition of this auxiliary agent is far smaller than the standard of the additive dosage of Europe requirement less than 4 weight % about 0.8 weight %.Disperser composition provided by the invention is no matter be can both use in wet method or when dry production iron phthalein is green.Specific performance index according to the green dispersant special of iron phthalein of the present invention preparation is as follows:
Outward appearance: colourless transparent liquid;
Solid content: 40 ± 2 weight %;
PH value: 6.0～7.0;
Viscosity: 100～400mPas;
Solvability in the water: molten entirely.
To be mixed with the slurry that solid content is 65～70 weight % with ferric oxide bloom and a certain amount of water by the phthalocyanine blue pigment after the dispersion agent modification provided by the invention, mediated 1 hour through kneader, can obtain the green color of iron phthalein, slurry grinds after the drying room oven dry and makes the green finished product of iron phthalein, after testing, performance is as follows:
Pigment water solubles content: 0.6 weight %; Not color separation of the green suspension liquid of iron (leaving standstill 24h); Making cement products does not whiten.
Embodiment
Below in conjunction with embodiment the present invention is further described in detail, but the present invention is in no way limited to these embodiment, wherein with " % " expression numerical value except that special instruction person, be " weight % ".
Embodiment 1
In beaker, it is stand-by that stirring and dissolving evenly obtains mix monomer with vinylformic acid 14g, butyl acrylate 3g, Isooctyl acrylate monomer 4g, N hydroxymethyl acrylamide 3g, ethoxylation propylene 1g weighing.Ammonium Persulfate 98.5 0.5g adding 5g deionized water for stirring dissolving back is stand-by.The deionized water, the intensification that add 33.5g in the 1000ml four-hole boiling flask of condenser, electric mixer, thermometer, dropping funnel is housed are stirred, when temperature rises to 82 ℃, beginning drips initiator and mix monomer simultaneously, keep temperature of reaction at 86～90 ℃, 4～6h drips off, and drips off back insulation 1h.The liquid caustic soda that slowly adds 26g30% behind the 1h adds and stirs 20min, adds polyoxyethylene octylphenol ether 10g and stirs, and 100 orders filter discharging and obtain dispersion agent.Product is a colourless transparent liquid, solid content 38%, and pH value 6.0, viscosity is 100mPas, molten entirely in water.
Embodiment 2
In beaker, it is stand-by that stirring and dissolving evenly obtains mix monomer with 2-butylene acid 15g, 2-butylene acid butyl ester 4g, 2-butylene acid different monooctyl ester 4.5g, acrylamide 4g, ethyl vinyl ether 1.5g weighing.Add in the above-mentioned mix monomer dibenzoyl peroxide 0.75g stand-by after the stirring and dissolving.The deionized water, the intensification that add 31.25g in the 1000ml four-hole boiling flask of condenser, electric mixer, thermometer, dropping funnel is housed are stirred, when temperature rises to 82 ℃, beginning drips initiator and mix monomer simultaneously, keep temperature of reaction at 86～90 ℃, 4～6h drips off, and drips off back insulation 1h.The liquid caustic soda that slowly adds 28g30% behind the 1h adds and stirs 20min, adds polyoxyethylene nonylphenol ether 11g and stirs, and 100 orders filter discharging and obtain dispersion agent.Product is colourless transparent liquid, solid content 40%, and pH value 6.5, viscosity is 250mPampas, molten entirely in water.
Embodiment 3
In beaker, it is stand-by that stirring and dissolving evenly obtains mix monomer with 2-methyl-2-pentenoic acid 16g, 2-methyl-2-pentenoic acid butyl ester 5g, the different monooctyl ester 5g of 2-methyl-2-pentenoic acid, N-N-isopropylacrylamide 5g, ethoxylation propylene 2g weighing.Add in the above-mentioned mix monomer Diisopropyl azodicarboxylate 1g stand-by after the stirring and dissolving.The deionized water, the intensification that add 24g in the 1000ml four-hole boiling flask of condenser, electric mixer, thermometer, dropping funnel is housed are stirred, when temperature rises to 82 ℃, beginning drips initiator and mix monomer simultaneously, keep temperature of reaction at 86～90 ℃, 4～6h drips off, and drips off back insulation 1h.The liquid caustic soda that slowly adds 30g30% behind the 1h adds and stirs 20min, adds polyoxyethylene octylphenol ether 12g and stirs, and 100 orders filter discharging and obtain dispersion agent.Product is colourless transparent liquid, solid content 42%, and pH value 7.0, viscosity is 400mPas, molten entirely in water.
Claims (3)
1. a special dispersant compound for iron phthalein green is characterized in that in weight percent, and the composition of said composition comprises:
Unsaturated fatty acids 10～20
Unsaturated fatty acid ester A 1～5
Unsaturated fatty acid ester B 1～5
Unsaturated amides 1～5
Functional monomer 1～5
Initiator 0.1～1
Liquid caustic soda 20～40
Alkylphenol polyoxyethylene 10～15,
At last, add to 100 weight % with deionized water;
Unsaturated fatty acids is selected from a kind of in vinylformic acid, 2-butylene acid, 3-butenoic acid, the acid of 3-methyl-2-butene, the 2-methyl-2-pentenoic acid;
Unsaturated fatty acid ester A is selected from a kind of in Butyl acrylate, 2-butylene acid butyl ester, 3-butyl crotonate, 3-methyl-2-butene acid butyl ester, the 2-methyl-2-pentenoic acid fourth fat;
Unsaturated fatty acid ester B is selected from a kind of in the different monooctyl ester of Isooctyl acrylate monomer, 2-butylene acid, the different monooctyl ester of 3-butenoic acid, the different monooctyl ester of 3-methyl-2-butene acid, the 2-methyl-different monooctyl ester of 2-pentenoic acid;
Unsaturated amides is selected from a kind of in acrylamide, N hydroxymethyl acrylamide, N,N-DMAA, the N-N-isopropylacrylamide;
Functional monomer is selected from a kind of in ethoxylation propylene or the ethyl vinyl ether;
Initiator is selected from a kind of in Ammonium Persulfate 98.5, dibenzoyl peroxide, tert-butyl peroxide hydrogen, the Diisopropyl azodicarboxylate;
Alkylphenol polyoxyethylene is selected from a kind of in polyoxyethylene octylphenol ether, the polyoxyethylene nonylphenol ether.
2. special dispersant compound for iron phthalein green according to claim 1, it is characterized in that each main component in the said composition in the use level of percentage is: unsaturated fatty acids 14～16%, unsaturated fatty acid ester A 3～5%, unsaturated fatty acid ester B 4～5%, unsaturated amides 3～5%, functional monomer 1～2%, initiator 0.5～1%.
3. the preparation method according to claim 1 or 2 described special dispersant compound for iron phthalein green is characterized in that whole process of preparation comprises the following steps:
(1) by after the proportioning weighing unsaturated fatty acids, unsaturated fatty acid ester A, unsaturated fatty acid ester B, unsaturated amides, functional monomer being placed container, stirring and dissolving is even, and it is stand-by to obtain mix monomer;
(2) initiator is added in appropriate amount of deionized water or the monomer stand-by after the stirring and dissolving;
(3) in the reaction vessel that condenser, electric mixer, thermometer, dropping funnel are housed, add proper amount of deionized water, heat up and stir, when temperature rises to 82 ℃, beginning drips ready initiator and mix monomer simultaneously, keep temperature of reaction at 86～90 ℃, 4～6h drips off, drip off back insulation 0.5～1.5h, slowly add liquid caustic soda then, add and stir 15～25min, the alkylphenol polyoxyethylene that adds formula ratio stirs, and 100 orders filter discharging and obtain described disperser composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100384730A CN101275038B (en) | 2007-03-26 | 2007-03-26 | Special dispersant compound for iron phthalein green and preparation thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007100384730A CN101275038B (en) | 2007-03-26 | 2007-03-26 | Special dispersant compound for iron phthalein green and preparation thereof |
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| Publication Number | Publication Date |
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| CN101275038A CN101275038A (en) | 2008-10-01 |
| CN101275038B true CN101275038B (en) | 2011-10-19 |
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| CN2007100384730A Expired - Fee Related CN101275038B (en) | 2007-03-26 | 2007-03-26 | Special dispersant compound for iron phthalein green and preparation thereof |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104761928A (en) * | 2014-01-08 | 2015-07-08 | 浙江德清美史乐颜料科技有限公司 | Green pigment and production process thereof |
| CN104497640A (en) * | 2014-12-26 | 2015-04-08 | 常熟洛克伍德颜料有限公司 | Preparation method of phthalocyanine blue-coated iron oxide yellow composite pigment |
| CN113622207B (en) * | 2021-07-28 | 2023-06-20 | 沂水祥腾化工有限公司 | Dispersing agent with glossiness for textile dye and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664018A (en) * | 2005-02-24 | 2005-09-07 | 上海一品国际颜料有限公司 | Sunfast ferro phthalocyanine green pigment for concrete and mortar and method for preparing same |
| CN1854103A (en) * | 2005-04-28 | 2006-11-01 | 上海一品国际颜料有限公司 | Improvement of iron phthaleinzurine fading in concrete products |
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- 2007-03-26 CN CN2007100384730A patent/CN101275038B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664018A (en) * | 2005-02-24 | 2005-09-07 | 上海一品国际颜料有限公司 | Sunfast ferro phthalocyanine green pigment for concrete and mortar and method for preparing same |
| CN1854103A (en) * | 2005-04-28 | 2006-11-01 | 上海一品国际颜料有限公司 | Improvement of iron phthaleinzurine fading in concrete products |
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Owner name: SHANGHAI HUAYI FINE CHEMICAL INDUSTRY CO., LTD. Free format text: FORMER OWNER: SHANGHAI CHANGFENG CHEMICAL FACTORY OF SHANGHAI COATINGS CO., LTD. Effective date: 20150506 |
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