CN1250813C - Cationic gum rosin sizing agent emulsion and method for preparing same - Google Patents
Cationic gum rosin sizing agent emulsion and method for preparing same Download PDFInfo
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- CN1250813C CN1250813C CNB2003101064549A CN200310106454A CN1250813C CN 1250813 C CN1250813 C CN 1250813C CN B2003101064549 A CNB2003101064549 A CN B2003101064549A CN 200310106454 A CN200310106454 A CN 200310106454A CN 1250813 C CN1250813 C CN 1250813C
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Abstract
The present invention relates to emulsion of a cation type rosin glue sizing agent, which is prepared by compounding anion rosin glue sizing agent emulsion and a cationization agent, wherein the cationization agent is prepared by polymerizing allyl monomers containing C=O carbonyls, polymer of which the molecular weight is from 20000 to 2000000 is obtained by cationization modification, the anion rosin glue sizing agent emulsion accounts for 50% to 95 wt%, and the cationization agent accounts for 5 to 50 wt%. The preparation method of the emulsion of the cation type rosin glue sizing agent comprises: adding allyl monomers containing C=O and a solvent of which the weight ratio is from 50% to 1000%(the allyl monomer is the reference) in a container, regulating the pH value from 3 to 7, raising the temperature from 35 DEG C to 70 DEG C, adding an initiating agent of which the weight ratio is from 0.01% to 5%, raising the temperature from 60 DEG C to 95 DEG C, keeping the temperature not less than 0.5h, reducing the temperature from 0 DEG C to 35 DEG C to obtain the polymer, carrying out the cationization modification to the polymer to obtain the cationization agent of which the molecular weight is from 20000 to 2000000, taking anion rosin sizing agent emulsion of which the weight percentage is from 50% to 95%, and adding the cationization agent of which the weight ratio is from 5 to 50% into the anion rosin glue sizing agent emulsion.
Description
Technical field:
The present invention relates to a kind of rosin sizing agent and preparation method thereof, particularly relate to a kind of cationic rosin sizing agent and preparation method thereof.
Background technology:
Because in/alkaline paper-making has and improves paper durability, reduces environmental pollution, alleviates plurality of advantages such as equipment corrosion, paper industry just by acid papermaking in/alkaline paper-making changes, this is a modern International Paper Developing Trend in Technology.Cationic dispersion rosin size can be adsorbed in electronegative fiber surface certainly, only need a small amount of alumina just can be implemented in papermaking under the nearly neutrallty condition, thereby numerous in recent years scientific research personnel is devoted to development, the development and application of cationic dispersion rosin size.Carrying out a lot of research work aspect the cationic rosin jelly both at home and abroad, be base stock mainly at present by rosin or fortified rosin, the water-soluble cationic material that is equipped with proper proportion makes, as: Canadian Patent 1045735, Canadian Patent 107149700, Canadian Patent 2081786, United States Patent (USP) 5817214 etc.And China existing how tame anion rosin milk manufacturer, with anion rosin milk cation colophony emulsion transition, not only processing ease is realized, and does not need big equipment input, has more realistic meaning.At present domestic have several families that the legal system that makes the transition is equipped with the unit that cation colophony size is studied, as: northwest light industry institute, Nanjing Forestry University, Shandong paper industry studying and designing institute etc., but aluminium salt consumption is excessive, or adopting expensive chloropropylene oxide is that resin etc. is cationic agent, improved production cost greatly, brought difficulty to practical application.
Summary of the invention:
The purpose of this invention is to provide a kind of low cost of manufacture and can improve anti-cloudy heteroion interference performance, can be used for general paper sizing under the neutrallty condition, be particularly useful for the Colophonium paper size latex emulsion of cationic and its preparation method of the high stuff sizing of beating degree.
Technical scheme of the present invention is:
A kind of cationic rosin sizing agent emulsion, the white emulsion that is composited by anion rosin sizing agent emulsion and cationic agent, this cationic agent is to be polymerized by a kind of vinyl monomer of the C=O of containing carbonyl at least, and behind cation modifying, obtain, molecular weight is the polymer of 20000-2000000, the shared percentage by weight of above-mentioned anion rosin sizing agent emulsion is 50%-95%, and the shared percentage by weight of cationic agent is 5-50% (by a solid content).
A kind of preparation method of cationic rosin sizing agent emulsion, the first step: in container, add at least a vinyl monomer that contains C=O, the solvent of percentage by weight 50%-1000% (is benchmark with the vinyl monomer), regulate the pH value to 3-7, be warming up to 35 ℃-70 ℃, add percentage by weight 0.01%-5% initator, be warming up to 60 ℃-95 ℃ again, keep being not less than 0.5h, be cooled to 0 ℃-35 ℃ and obtain polymer, then polymer is carried out cation modifying, get cationic agent, molecular weight is 20000-2000000, and second step: getting percentage by weight is 50%-95% anion rosin sizing agent emulsion, with percentage by weight is that the cationic agent (all by solid content) of 5-50% adds wherein, stirs simultaneously.
Beneficial effect of the present invention: cationic rosin sizing agent cost provided by the invention is low, anti-cloudy heteroion disturbs, can be used for general paper sizing under the neutrallty condition, be particularly useful for the applying glue of the high paper pulp of beating degree, for example, when being slurry with the import softwood pulp, the sizing efficiency of this product be the sizing efficiency basically identical of the sizing agent of cationic agent with polyamide polyamine chloropropylene oxide resin, and when being slurry with the regenerated paper pulp, it is the sizing efficiency of the sizing agent of cationic agent that the sizing efficiency of this product is better than with polyamide polyamine chloropropylene oxide resin far away, the high 10-30s of degree of sizing, regenerated paper pulp is the recycling of waste paper, waste paper need be handled as the deinking of deinking agent through anionic surfactant, anion can remain in the regenerated paper pulp of making, and cationic size is caused interference, and this product is when being slurry with the regenerated paper pulp, sizing efficiency is better than contrast product far away, illustrates that the antijamming capability of this product is strong; The preparation method of cationic rosin sizing agent provided by the invention is simple, cost of equipment is low, easy operating, production cost is low, ratio is epichlorohydrin resins product price transition low 40% in the past, for example, the cost of the cationic rosin sizing agent of this product is 6000 yuan/ton, and is that the cost of the sizing agent of cationic agent is 10000 yuan/ton (by 100% solid contents) in polyamide polyamine chloropropylene oxide resin.
The specific embodiment:
Embodiment 1
In having the 250ml four-hole boiling flask of agitator, thermometer, reflux condenser, add acrylic acid 50g, isopropyl alcohol 500g, stirring, is 6 with 10% hydrochloric acid adjust pH, is warmed up to 35 ℃, add ammonium persulfate 0.005g, be warming up to 80 ℃ of reaction temperatures then, keep 3.0h, reaction steams solvent after finishing, and is cooled to 25 ℃, add cation modifying agent epoxychloropropane 12g then, tertiary amine (as triethylamine) 15g is heated to 95 ℃, keep 2h, be cooled to 35 ℃, get modified cationized dose; Get 50% anionic rosin milk 30g, add synthesis modification cationic agent 1g, stir, add cationic starch 0.5g, under 5 ℃, finish the electrical transition process of emulsion, get finished product.Product is used for degree of sizing to be measured, and the pH value is 6.0, and alumina and sizing agent consumption are at 1.0% o'clock, and the degree of sizing of page is 45s.
Embodiment 2
In having the 250ml four-hole boiling flask of agitator, thermometer, reflux condenser, add methacrylic acid 25g, acryloyl quaternary ammonium salt 25g, water 150g stirs, with 10% hydrochloric acid adjust pH is 5, be warmed up to 45 ℃, add ammonium persulfate 2.5g, be warming up to 90 ℃ of reaction temperatures then, keep 1.5h, reaction steams solvent after finishing, and is cooled to 15 ℃, add cation modifying agent epoxychloropropane 6g then, tertiary amine (as triethylamine) 7g is heated to 70 ℃, keeps 6h, be cooled to 20 ℃, get modified cationized dose; In equipment container with stirring, heating, thermometric, reflux condensate device, add butyl acrylate 50g, solvent toluene 25g stirs, be warmed up to 80 ℃, add ammonium persulfate 0.005g, be warming up to 95 ℃ of reaction temperatures then, keep 1h, after reaction finishes, concentrate, cool to 35 ℃, promptly obtain can be used as the polyalkenes material of stabilizing agent; Get 50% anionic rosin milk 30g, add stabilizing agent 3.0g, stir, and then add synthesis modification cationic agent 3g, and stir, adding molecular weight is 2000000 cationic polyacrylamide 0.1g, under 25 ℃, finish the electrical transition process of emulsion, get finished product.Product is used for degree of sizing to be measured, and the pH value is 6.0, and alumina and sizing agent consumption are at 1.0% o'clock, and the degree of sizing of page is 55s.
Embodiment 3
In having the 250ml four-hole boiling flask of agitator, thermometer, reflux condenser, add acrylamide 30g, maleic anhydride 20g, isopropyl alcohol 25g stirs, with 10% hydrochloric acid adjust pH is 6.5, be warmed up to 65 ℃, add potassium peroxydisulfate 1.0g, be warming up to 60 ℃ of reaction temperatures then, keep 5.0h, reaction steams solvent after finishing, and is cooled to 5 ℃, add cation modifying agent epoxychloropropane 9g then, tertiary amine (as triethylamine) 11g is heated to 80 ℃, keeps 4h, be cooled to 5 ℃, get modified cationized dose; In equipment container, add acrylic acid 25g, methacrylic acid 25g with stirring, heating, thermometric, reflux condensate device, solvent isopropyl alcohol 300g, stir, be warmed up to 55 ℃, add cerous nitrate 1.0g, be warming up to 80 ℃ of reaction temperatures then, keep 3h, after reaction finishes, concentrate, cool to 15 ℃, promptly obtain can be used as the polyalkenes material of stabilizing agent; Get 50% anionic rosin milk 30g, thin up, add stabilizing agent 6.0g, stir, and then add synthesis modification cationic agent 9g, adding molecular weight is 2000000 cationic polyamide epoxy polyamine chloropropane 0.5g, stirs, under 10 ℃, finish the electrical transformation of emulsion, get finished product.Product is used for degree of sizing to be measured, and the pH value is 6.5, and alumina and sizing agent consumption are at 1.0% o'clock, and the degree of sizing of page is 74s.
Embodiment 4
In having the 250ml four-hole boiling flask of agitator, thermometer, reflux condenser, add maleic acid 45g, styrene 5g, toluene 150g stirs, with 10% hydrochloric acid adjust pH is 3.5, be warmed up to 55 ℃, add cerous nitrate 0.1g, be warming up to 95 ℃ of reaction temperatures then, keep 0.5h, reaction steams solvent after finishing, and is cooled to 0 ℃, with NaOH 10% aqueous solution pH value is adjusted to 10, add clorox 10g, be heated to 70 ℃ then, keep 6h, be cooled to 0 ℃, get modified cationized dose; In equipment container, add acrylamide 45g, methyl methacrylate 5g with stirring, heating, thermometric, reflux condensate device, aqueous solvent 500g, stir, be warmed up to 40 ℃, add potassium peroxydisulfate 2.5g, be warming up to 60 ℃ of reaction temperatures then, keep 6h, after reaction finishes, concentrate, cool to 5 ℃, promptly obtain can be used as the polyalkenes material of stabilizing agent; Get 50% anionic rosin milk 30g, thin up adds stabilizing agent 1.0g, stirs, and then adds synthesis modification cationic agent 15g, adds casein 0.5g, stirs, and finishes the electrical transition process of emulsion under 5 ℃, gets finished product.Product is used for degree of sizing to be measured, and the pH value is 6.0, and alumina and sizing agent consumption are at 1.0% o'clock, and the degree of sizing of page is 55s.
Embodiment 5
In having the 250ml four-hole boiling flask of agitator, thermometer, reflux condenser, add acrylamide 30g, acryloyl quaternary ammonium salt 5g, methyl methacrylate 15g, water 25g, stirring, is 4 with 10% hydrochloric acid adjust pH, is warmed up to 40 ℃, add ammonium persulfate 0.05g, be warming up to 85 ℃ of reaction temperatures then, keep 2.0h, after reaction finishes, steam solvent, be cooled to 35 ℃, the pH value be adjusted to 10, add clorox 30g with NaOH 10% aqueous solution, be heated to 95 ℃ then, keep 2h, be cooled to 35 ℃, get modified cationized dose; In equipment container with stirring, heating, thermometric, reflux condensate device, add acrylamide 50g, aqueous solvent 150g stirs, be warmed up to 80 ℃, add cerous nitrate 2.5g, be warming up to 100 ℃ of reaction temperatures then, keep 6h, after reaction finishes, concentrate, cool to 5 ℃, promptly obtain can be used as the polyalkenes material of stabilizing agent.Get 50% anionic rosin milk 30g, thin up adds stabilizing agent 4.0g, stirs, and then adds synthesis modification cationic agent 12g, stirs, and finishes the electrical transition process of emulsion under 35 ℃, gets finished product.Product is used for degree of sizing to be measured, and the pH value is 6.0, and alumina and sizing agent consumption are at 1.0% o'clock, and the degree of sizing of page is 52s.
Embodiment 6
Has agitator, thermometer, in the 250ml four-hole boiling flask of reflux condenser, add acrylamide 30g, acryloyl quaternary ammonium salt 5g, methyl methacrylate 15g, water 25g stirs, with 10% hydrochloric acid adjust pH is 4, is warmed up to 40 ℃, adds ammonium persulfate 0.05g, be warming up to 85 ℃ of reaction temperatures then, keep 2.0h, reaction steams solvent after finishing, be cooled to 35 ℃, with NaOH 10% aqueous solution pH value is adjusted to 10, adds clorox 30g, be heated to 95 ℃ then, with NaOH 10% aqueous solution pH value is adjusted to 10, add clorox 20g, be heated to 85 ℃ then, keep 4h, be cooled to 35 ℃, get modified cationized dose; Get 50% anionic rosin milk 30g, thin up stirs, and then adds synthesis modification cationic agent 12g, stirs, and finishes the electrical transition process of emulsion under 35 ℃, gets finished product.Product is used for degree of sizing to be measured, and the pH value is 6.0, and alumina and sizing agent consumption are at 1.0% o'clock, and the degree of sizing of page is 40s.
Embodiment 7
A kind of cationic rosin sizing agent emulsion, the white emulsion that is composited by anion rosin sizing agent emulsion and cationic agent, this cationic agent is to be polymerized by a kind of vinyl monomer of the C=O of containing carbonyl at least, and behind cation modifying, obtain, molecular weight is the polymer of 20000-2000000, the shared percentage by weight of above-mentioned anion rosin sizing agent emulsion is 50%-95%, the shared percentage by weight of cationic agent is 5-50% (all by a solid content), in the present embodiment, vinyl monomer is for containing
Vinyl monomer, contain
Vinyl monomer be acids, anhydrides, present embodiment adding epoxychloropropane and tertiary amine are as the cation modifying agent, can add percentage by weight in anionic rosin milk and cationic agent recombination process is that (with anion rosin sizing agent emulsion is benchmark to 0-40%, by solid content) the polyalkenes stabilizing agent, this polyalkenes stabilizing agent contains the C=O vinyl monomer by two kinds and is polymerized, molecular weight is 20000-2000000, and vinyl monomer can be acrylic acid, acrylamide, methacrylic acid, acrylate; Present embodiment adds percentage by weight 0-20% in anionic rosin milk and cationic agent recombination process (with anion rosin sizing agent emulsion is benchmark, by solid content) auxiliary agent, this auxiliary agent is at least by a kind of the combining in alkyl quaternary amine salt, cationic starch, polyacrylamide, cationic polyamide epoxy polyamine resin, the casein, the molecular weight of polymer wherein is 10000-2000000, the preferred cationic polyacrylamide.
Embodiment 8
A kind of cationic rosin sizing agent emulsion, the white emulsion that is composited by anion rosin sizing agent emulsion and cationic agent, this cationic agent is to be polymerized by a kind of vinyl monomer of the C=O of containing carbonyl at least, and behind cation modifying, obtain, molecular weight is the polymer of 20000-2000000, the shared percentage by weight of above-mentioned anion rosin sizing agent emulsion is 50%-95%, the shared percentage by weight of cationic agent is 5-50% (all by a solid content), in the present embodiment, vinyl monomer is for containing
Vinyl monomer, contain
Vinyl monomer can adopt amide-type, quaternary ammonium salt, be preferably maleic acid, maleic anhydride, acrylic acid, acrylamide, methacrylic acid, acryloyl quaternary ammonium salt; Present embodiment adds clorox or other hypochlorites are the cation modifying agent, adding percentage by weight in anionic rosin milk and cationic agent recombination process is that (with anion rosin sizing agent emulsion is benchmark to 0-40%, by solid content) the polyalkenes stabilizing agent, this polyalkenes stabilizing agent contains the C=O vinyl monomer by two kinds and is polymerized, molecular weight is 20000-2000000, and vinyl monomer can be acrylic acid, acrylamide, methacrylic acid, acrylate; Present embodiment adds percentage by weight 0-20% in anionic rosin milk and cationic agent recombination process (with anion rosin sizing agent emulsion is benchmark, by solid content) auxiliary agent, this auxiliary agent is at least by a kind of the combining in alkyl quaternary amine salt, cationic starch, polyacrylamide, cationic polyamide epoxy polyamine resin, the casein, the molecular weight of polymer wherein is 10000-2000000, the preferred cationic polyacrylamide.
Embodiment 9
The preparation method of cationic rosin sizing agent emulsion,
The first step: in container, add at least a vinyl monomer that contains C=O, the solvent of percentage by weight 50%-1000% (is benchmark with the vinyl monomer), this solvent is a known solvent in the vinyl monomer polymerisation, for example: water, the toluene class, b propanol etc., regulate pH value to 3-7, be warming up to 35 ℃-70 ℃, add percentage by weight 0.01%-5% initator, used initator is a known initator in the vinyl monomer polymerisation, for example: cerous nitrate, ammonium persulfate, potassium peroxydisulfate etc., be warming up to 60 ℃-95 ℃ again, keep being not less than 0.5h, be cooled to 0 ℃-35 ℃ and obtain polymer, then polymer is carried out cation modifying, get cationic agent, molecular weight is 20000-2000000, in order to promote the vinyl monomer polymerization, in the cationic agent compound process, can add styrene or the esters of acrylic acid of percentage by weight 0-50%
Second step: getting percentage by weight is 50%-95% anion rosin sizing agent emulsion, with percentage by weight is that the cationic agent (by solid content) of 5-50% adds wherein, stir simultaneously, get cationization rosin sizing agent emulsion, before anionic rosin milk and cationic agent mixed process, adding percentage by weight in anionic rosin sizing agent emulsion is the polyalkenes stabilizing agent of 0-40%, the polyalkenes stabilizing agent is to be polymerized by a kind of C=O of containing vinyl monomer at least, molecular weight is 20000-2000000, and adopt following method preparation: adding vinyl monomer and percentage by weight are the solvent of 50%-1000% (is benchmark with the vinyl monomer that is added) in container, add vinyl monomer this moment is polyacrylamide, phenylethylene etc., the solvent that is added is a known solvent in the vinyl monomer polymerisation, for example: water, the toluene class, b propanol etc., be warming up to 35 ℃-80 ℃, adding percentage by weight is the initator of 0.01%-5%, be warming up to 60 ℃-100 ℃, keep being not less than 0.5H, be cooled to 0 ℃-35 ℃, obtain the polyalkenes stabilizing agent, in the present embodiment, the polyalkenes stabilizing agent is polymerized by two kinds of vinyl monomers, in the white emulsion that anionic rosin milk and cationic agent mix, add and contain percentage by weight 0-20% (with anion rosin sizing agent emulsion is benchmark, by solid content) auxiliary agent, this auxiliary agent is by the alkyl quaternary amine salt, cationic starch, polyacrylamide, cationic polyamide epoxy polyamine resin, a kind of combining in the casein, wherein the molecular weight of the polymer that is adopted is 10000-2000000, add stabilizing agent, can improve sizing agent emulsion stability, electropositive, anti-assorted anion interference capability is to improve the dispersiveness of sizing agent emulsion.
Claims (7)
1, a kind of cationic rosin sizing agent emulsion, it is characterized in that in the anion rosin milk, adding earlier in anion rosin sizing agent emulsion be benchmark and by the percentage by weight of solid content for greater than 0 and less than 40% polyalkenes stabilizing agent, the white emulsion that is composited by anion rosin sizing agent emulsion and cationic agent again, this cationic agent is to be polymerized by a kind of vinyl monomer of the C=O of containing carbonyl at least, and behind cation modifying, obtain, molecular weight is the polymer of 20000-2000000, the shared percentage by weight of above-mentioned anion rosin sizing agent emulsion is 50%-95%, and the shared percentage by weight of cationic agent is counted 5-50% by solid content.
2,, it is characterized in that vinyl monomer is for containing according to the described sizing agent emulsion of claim 1
3, according to the described sizing agent emulsion of claim 1, it is characterized in that the polyalkenes stabilizing agent contains the C=O vinyl monomer by two kinds and is polymerized, molecular weight is 20000-2000000.
4, according to the described sizing agent emulsion of claim 1, it is characterized in that in anionic rosin milk and the cationic agent mixed process adding in anion rosin sizing agent emulsion be benchmark and by the percentage by weight of solid content for greater than 0 and less than 20% auxiliary agent, at least by a kind of composition the in alkyl quaternary amine salt, cationic starch, polyacrylamide, cationic polyamide epoxy polyamine resin, the casein, the molecular weight of polymer wherein is 10000-2000000 to this auxiliary agent.
5, a kind of preparation method who is used to implement the described cationic rosin sizing agent emulsion of claim 1 is characterized in that:
The first step: in container, add at least a vinyl monomer that contains C=O, with the vinyl monomer is the solvent of the percentage by weight 50%-1000% of benchmark, regulates the pH value to 3-7, is warming up to 35 ℃-70 ℃, adding is the percentage by weight 0.01%-5% initator of benchmark with the vinyl monomer, be warming up to 60 ℃-95 ℃ again, keep being not less than 0.5h, be cooled to 0 ℃-35 ℃ and obtain polymer, then polymer is carried out cation modifying, get cationic agent, molecular weight is 20000-2000000
Second step: getting percentage by weight is 50%-95% anion rosin sizing agent emulsion, in anionic rosin sizing agent emulsion, add earlier in anion rosin sizing agent emulsion be benchmark and by the percentage by weight of solid content for greater than 0 and less than 40% polyalkenes stabilizing agent, with being that the cationic agent of 5-50% adds wherein all, stir simultaneously by the percentage by weight of solid content.
6, the preparation method of cationic rosin sizing agent emulsion according to claim 5, it is characterized in that the polyalkenes stabilizing agent is to be polymerized by a kind of C=O of containing vinyl monomer at least, molecular weight is 20000-2000000, and adopt following method preparation: adding vinyl monomer and percentage by weight are the solvent of 50%-1000% in container, be warming up to 35 ℃-80 ℃, adding is that the percentage by weight of benchmark is the initator of 0.01%-5% with the vinyl monomer that is added, be warming up to 60 ℃-100 ℃, keep being not less than 0.5H, be cooled to 0 ℃-35 ℃, obtain the polyalkenes stabilizing agent.
7, the preparation method of cationic rosin sizing agent emulsion according to claim 5, it is characterized in that in the white emulsion that anionic rosin milk and cationic agent mix, can adding in anion rosin sizing agent emulsion be benchmark and by the solid content percentage by weight greater than 0 and less than 20% auxiliary agent, at least by a kind of composition the in alkyl quaternary ammonium salts, cationic starch, polyacrylamide, cationic polyamide epoxy polyamine resin, the casein, wherein the molecular weight of the polymer that is adopted is 10000-2000000 to this auxiliary agent.
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| CNB2003101064549A CN1250813C (en) | 2003-11-28 | 2003-11-28 | Cationic gum rosin sizing agent emulsion and method for preparing same |
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| CNB2003101064549A CN1250813C (en) | 2003-11-28 | 2003-11-28 | Cationic gum rosin sizing agent emulsion and method for preparing same |
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| CN1295014C (en) * | 2005-05-23 | 2007-01-17 | 山东轻工业学院 | Cationic dispersion rosin size |
| CN101400853B (en) * | 2006-03-30 | 2011-07-27 | 播磨化成株式会社 | Cationic surface sizing agent and paper coated with the sizing agent |
| CN107476125A (en) * | 2017-09-18 | 2017-12-15 | 江苏亘德科技有限公司 | A kind of rosin sizing agent and preparation method thereof |
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Assignee: Jiangxi Jin'an Forestry Industrial Co., Ltd. Assignor: Institute of Chemical Industry of Forest Products, Chinese Academy of Forestry Contract fulfillment period: 2009.3.10 to 2013.12.31 contract change Contract record no.: 2009360000018 Denomination of invention: Cationic gum rosin sizing agent emulsion and method for preparing same Granted publication date: 20060412 License type: Exclusive license Record date: 2009.4.14 |
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