CN105315757B - Organic silicon leveling agent and preparation method thereof - Google Patents
Organic silicon leveling agent and preparation method thereof Download PDFInfo
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- CN105315757B CN105315757B CN201510891948.5A CN201510891948A CN105315757B CN 105315757 B CN105315757 B CN 105315757B CN 201510891948 A CN201510891948 A CN 201510891948A CN 105315757 B CN105315757 B CN 105315757B
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Abstract
The invention relates to the field of high molecular materials and in particular relates to an organic silicon leveling agent and a preparation method thereof. The organic silicon leveling agent is polyether-polyester modified organosiloxane and has a structure as shown in the specification, wherein R=H or R=CH3; or the organic silicon leveling agent has another structure as shown in the specification, wherein R1=-CH3, C2H5 or C3H7; x is 8-14; y is 3-8; and m is 20-200, n is 30-100, and the sum of n and m is 50-250. The organic silicon leveling agent belongs to polyether-polyester modified organosiloxane and has favorable leveling property and stability. The invention also provides the preparation method of the organic silicon leveling agent, which is convenient for industrial production.
Description
Technical field
The present invention relates to polymeric material field, more specifically to a kind of organosilicon levelling agent and preparation method thereof.
Technical background
Levelling agent is conventional coating additive, it can promote coating formed during drying and forming-film one smooth, smooth,
Uniform film.Covering with paint liquid surface tension can effectively be reduced, improve a class material of its levelability and uniformity.Covering with paint can be improved
The permeability of liquid, can reduce the probability producing speckle and spot when brushing, increase spreadability, make film forming uniform, natural.According to
The difference of chemical constitution, this kind of levelling agent mainly has three major types: acrylic compounds, silicone and fluorocarbons class.
Polyether polyester azo polyether polyeste belongs to the organopolysiloxane of pectinate texture.Its compatibility be rely on polyethers and
, come to adjust, the longer compatibility of chain is better for polyester.Polyether-modified most of this apoplexy due to endogenous wind, are usually used oxirane and epoxy third
Alkane.Oxirane and expoxy propane can be used alone it is also possible to be used in mixed way, and use it to control hydrophilic, lipophile.If with
Shi Hanyou ethyoxyl and propoxyl group, are just made for the levelling agent of the type siloxane of Water/oil dual-purpose.Molecular weight is bigger, its apparent condition
Control ability is stronger, and increasing slip, resistance to blocking are better.Modified polyester or polyethers are linked with two kinds of sides with siloxanes
A kind of method: siliconoxygen bond；Another kind is silicon-carbon chain, and in general, it is good that the former heat stability and resistance to water are not so good as the latter.With gathering
The compatibility of ether, polyester modification siloxanes and resin is greatly improved, and reduces surface tension, the energy of control surface flowing
Power, the slip that increases, nonshrink hole, tissue adhesion effect also all fine, individual product also has ply adhesion problem.Especially polyethers changes
The polysiloxanes of property, heat stability is bad, easily surely steeps.
Content of the invention
(1) technical problem to be solved
The present invention, on the basis of having drawn forefathers' research experience, is devoted to providing a kind of organosilicon levelling agent, this is organic
Silicon levelling agent belongs to polyether polyester azo polyether polyeste, has good levelability and stability, and another object is to provide
Its preparation method, is easy to industrialized production.
(2) technical scheme
The present invention provides a kind of organosilicon levelling agent, and described organosilicon levelling agent is polyether polyester modified organic silicon oxygen
Alkane.
The structure of described organosilicon levelling agent is
Wherein, r=h, or r=ch3, orOrr1=-ch3、c2h5、c3h7；
Described x value is 8-14；Y value is 3-8；M value is 20-200, and n value is 30-100, and n+m is 50-250.
A kind of preparation method of organosilicon levelling agent, is characterized in that: the synthesis of described organosilicon levelling agent is by side chain
Containing hydrogen silicone oil a, allyl polyether b are reacted,
Wherein, r=h, or r=ch3, orOrr1=-ch3、c2h5、c3h7；
Described x value is 8-14；Y value is 3-8；M value is 20-200, and n value is 30-100, and n+m is 50-250.
A kind of preparation method of organosilicon levelling agent, can heat and the reaction vessel that stirs in add solvent, will be described
Side chain containing hydrogen silicone oil a 30-60 weight portion, with described allyl polyether b 70-160 weight portion under the conditions of 60 DEG C -90 DEG C, stirs
Mix reaction 1-3 hour, be prepared into polyether polyester azo polyether polyeste；Described solvent is dimethylbenzene, butyl acetate, methyl tert-butyl
The mixing of one or more of base ketone.
Described organosilicon levelling agent is as the purposes of levelling agent.
Described organosilicon levelling agent is as the purposes for coating, the levelling agent of printing-ink.
The polymer of method of the present invention preparation, has extremely low surface tension, compares with common levelling agent, have lower
Foam stability, the polymer of the present invention, can for solid form it is also possible to be dissolved in organic solvent or water it is also possible to neutralization after
It is dissolved in water.This polymer is added to organic solvent type coatings system, aqueous coating system it is also possible to and inorganic carrier, such as titanium dioxide
Silicon, kieselguhr or aluminium oxide etc., make powder levelling agent, are added in powdery paints, play the effect of levelling.
Specific embodiment
For making the object, technical solutions and advantages of the present invention of greater clarity, with reference to specific embodiment, to this
Invention further describes.It should be understood that these descriptions are simply exemplary, and it is not intended to limit the scope of the present invention.This
Outward, in the following description, eliminate the description to known features and technology, to avoid unnecessarily obscuring idea of the invention.
Embodiment 1
Add dimethylbenzene 180g in there-necked flask, side chain containing hydrogen silicone oil a 30g, with described pi-allyl under the conditions of 60 DEG C
Polyethers b 70g, stirring reaction 3 hours, it is prepared into polyether polyester azo polyether polyeste, fundamental reaction is complete.Obtain transparent
Pale yellow solution, gpc test molecule amount, mn=36912, pdi=1.21.
Example 2
Add dimethylbenzene 350g in there-necked flask, side chain containing hydrogen silicone oil a 60g, with described pi-allyl under the conditions of 60 DEG C
Polyethers b 160g, stirring reaction 1.5 hours, it is prepared into polyether polyester azo polyether polyeste, fundamental reaction is complete.Obtain transparent
Pale yellow solution, gpc test molecule amount, mn=8959, pdi=1.23.
Example 3
Add butyl acetate 200g in there-necked flask, side chain containing hydrogen silicone oil a 200g, with described alkene under the conditions of 60 DEG C
Propyl group polyethers b 500g, stirring reaction 2.5 hours, it is prepared into polyether polyester azo polyether polyeste, fundamental reaction is complete.Obtain
Transparent pale yellow solution, gpc test molecule amount mn=57000, pdi=1.26.
Example 4
Add methyl iso-butyl ketone (MIBK) 300g in there-necked flask, side chain containing hydrogen silicone oil a 500g, with institute under the conditions of 60 DEG C
State allyl polyether b 1500g, stirring reaction 3 hours, be prepared into polyether polyester azo polyether polyeste, fundamental reaction is complete.
Obtain lurid clear solution.Gpc test molecule amount, mn=100315, pdi=1.38.
Embodiment 5
Table 1: the formula of powdery paints
Evaluation condition:
With agitator, each component is mixed.Then mixture is 95 DEG C in inlet temperature, and outlet temperature is 110 DEG C of powder
Extrude in extruder, be then passed through tablet machine tabletted.Pulverize through pulverizer again, then pass through the screen filtration of 200 mesh
Become finished powder coating.Under 60kv using esb-wagner corona cup gun by finished powder compositionss electrostatic spraying to aluminum
Plate up to coating thickness is 55～65um.The plate of coating is solidified 10 minutes in 200 DEG C of electric oven.
Mensure following parameters:
1st, use byk gardner mist shadow glossometer (haze-gloss) in the glossiness of 20 ° of measurements.High glaze angle value represents
Film has high reflectance.
2nd, the image definition (doi) being measured with byk gardner orange peel instrument (wave-scan doi).When doi value is for 0,
Diffuse-reflectance is optimal；Doi value means perfect mirror image for 100, and it represents the surface of unusual light.
3rd, byk gardner orange peel instrument is used to measure long wave.The long wave number of lesser amt represents the more smooth coating of outward appearance.
Table 2: the result after solidifying 10 minutes at 200 DEG C
| Levelling agent | 20 ° of glossiness | Long wave | Shortwave | doi |
| Business levelling agent | 83 | 60 | 46 | 79 |
| Embodiment 1 | 95 | 52 | 41 | 87 |
| Embodiment 2 | 87 | 53 | 38 | 85 |
| Embodiment 3 | 89 | 48 | 37 | 87 |
| Embodiment 4 | 93 | 51 | 41 | 88 |
Levelling agent embodiment 1 from this table as can be seen that in the present invention, embodiment 2, embodiment 3, embodiment 4 are relatively
There is higher levelling effect in business levelling agent, obtain more smooth surface.
The PVvalue testing of embodiment 6 baking vanish
Table 3: baking vanish formula
| Classification | Alkyd resin | Amino resin curing agents | Solvent | Amount to |
| Title | 3430 (domestic) | 582-2 (domestic) | Butyl acetate | |
| Weight (g) | 78 | 22 | 10 | 110 |
After raw material mixing in table, it is separately added into business levelling agent and example 1 and 4, is configured to baking vanish, is tested.
Baking vanish is scratched on a glass, room temperature is dried, then 125 DEG C of dryings 40 minutes again.Before measuring, coating is existed
Ambient temperature 24h.Tested with ray ran microprocessor system.The weight that machine carries 200g passes through coating, and measures quiet
State and dynamic coefficient of friction n.Result is as follows:
Can be seen that from these results, the static state of baking vanish and the dynamic coefficient of friction that comprise levelling agent configuration of the present invention are notable
Baking vanish less than the levelling agent configuration comprising routine.The polymer organic silicon levelling agent that generally present invention is obtained is than conventional levelling
The flow leveling of agent is more superior.
Claims (3)
1. a kind of organosilicon levelling agent is it is characterised in that the structure of described organosilicon levelling agent is
Its preparation method is: adds methyl iso-butyl ketone (MIBK) 300g in there-necked flask, side chain containing hydrogen silicone oil a 500g, in 60 DEG C of bars
With allyl polyether b 1500g under part, stirring reaction 3 hours, it is prepared into polyether polyester azo polyether polyeste, obtain light yellow
Clear solution, gpc test molecule amount, mn=100315, pdi=1.38,
.
2. organosilicon levelling agent according to claim 1 it is characterised in that: described organosilicon levelling agent is as levelling agent
Purposes.
3. organosilicon levelling agent according to claim 1 it is characterised in that: described organosilicon levelling agent is as applying
Material, the purposes of the levelling agent of printing-ink.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017033828A1 (en) * | 2015-08-24 | 2017-03-02 | Dic株式会社 | Ink composition for organic semiconductor elements, and organic semiconductor element using same |
| CN105585715A (en) * | 2016-03-03 | 2016-05-18 | 张耀忠 | Polyether modified organic silicon leveling agent |
| CN108047452B (en) * | 2017-12-20 | 2021-02-26 | 山东东岳有机硅材料股份有限公司 | Ultrahigh molecular weight polyether modified polysiloxane for leveling agent and preparation method and application thereof |
| CN108047805A (en) * | 2017-12-29 | 2018-05-18 | 陈鹏 | A kind of compound levelling agent and its preparation method and application |
| CN108192487B (en) * | 2018-01-29 | 2019-11-22 | 优美特（北京）环境材料科技股份公司 | It is a kind of to recoat the aqueous polyurethane finishing coat haveing excellent performance and preparation method |
| CN111040174B (en) * | 2018-10-15 | 2022-08-16 | 上海飞凯材料科技股份有限公司 | Polyether modified organic silicon acrylate, preparation method thereof and mold release agent |
| CN110128659B (en) * | 2019-05-15 | 2021-11-09 | 珠海东诚新材料股份有限公司 | Organic silicon flatting agent capable of improving coating recoating performance and application thereof |
| CN112111065A (en) * | 2020-08-13 | 2020-12-22 | 广东轻工职业技术学院 | Preparation method of polyether modified organic silicon flatting agent |
| CN116478359B (en) * | 2023-03-29 | 2024-04-16 | 宁波润禾高新材料科技股份有限公司 | Polysiloxane material for preventing jean fabric from losing elasticity, preparation method and application |
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| CN102643565B (en) * | 2012-05-04 | 2013-04-10 | 浙江润禾有机硅新材料有限公司 | Terminal modified organic silicone coating flatting agent and preparation method thereof |
| CN103214895B (en) * | 2013-04-26 | 2015-09-30 | 广东省石油化工研究院 | Organosilicon coating levelling agent and preparation method thereof |
| CN104592802B (en) * | 2013-10-30 | 2017-09-05 | 上海飞凯光电材料股份有限公司 | A kind of preparation method of organic silicon modified by polyether |
| CN104772074A (en) * | 2015-04-22 | 2015-07-15 | 浙江润禾有机硅新材料有限公司 | Hydrolysis-resistant organosilicon surface active agent and preparation method thereof |
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