CN103937001A - Method for preparing water-dispersible alkyl/polyether amino-silicon resin - Google Patents
Method for preparing water-dispersible alkyl/polyether amino-silicon resin Download PDFInfo
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Abstract
The invention discloses a method for preparing a water-dispersible alkyl/polyether amino-silicon resin. The method comprises the following steps of firstly carrying out a hydrosilation addition reaction on hydrogen-containing silicone resin, small molecular alkenyl epoxy compound and alpha-olefin according to a molar ratio of Si-H bond to alkylene group C=C double bond of 1: (1.0-1.5), synthesizing an alkyl/epoxy silicone resin intermediate and then carrying out an ammonolysis ring-opening reaction on the intermediate and polyether at 45-120 DEG C to obtain the alkyl/polyether amino-silicon resin. The alkyl/polyether amino-silicon resin prepared according to the invention can be dissolved or dispersed in water to form a stable silicon emulsion or microemulsion after the alkyl/polyether amino-silicon resin is diluted with a solvent, and thus the silicon resin is expected to be used for the field of a water-based finishing agent or a coating material.
Description
Technical field
The invention belongs to silicone resin field, being specifically related to a kind of water can emulsion dispersion type, be connected with the preparation method of the silicone resin of long alkyl chain length and polyethers amino group in structure simultaneously.
Background technology
Silicone resin taking Si-O-Si as main chain, side chain connects other organic groups, structure is highly cross-linked netted, the trapezoidal or isostructural siloxane polymer of semiclosed cage shape.Silicone resin has the dual nature of organic resin and inorganic materials concurrently, there is excellent heat-resistant stability, electrical insulating property, weather-proof water-repellancy, anti-salt fog, mould proof and biocompatibility, can be widely used in the fields such as aerospace, military project, electric, rubber plastic, leather, Material Processing and Modif ication.
In silicone resin, if connected organic group structure is different from kind, can there is notable difference in the performance of silicone resin, as epoxy group(ing) silicone resin, have both the over-all properties of epoxy compounds and silicone resin, can be heat-resisting, anticorrosion, oil resistant, protection against the tide, insulation, again can low-temperature curing, therefore the aspect such as anticorrosion and organic silicon insulating varnish preparation is widely used at high temperature resistant weather-resistant coating, high temperature service.And Silicon Containing Hydrogen resin and ethene silicone resin, because containing reactable Si-H key and vinyl group in structure, therefore can be used for the aspects such as the preparation of add-on type sulphurated siliastic, LED seal gum.
Silicone resin is scarcely water-soluble, is mainly used in oil soluble system, and this has limited the application of silicone resin in water-based system.At present, although synthetic about silicone resin a lot of with the research report of application both at home and abroad, there is not yet relevant water and dispersible the patent report of type alkyl/polyethers amino silicone.
Summary of the invention
The object of the invention is to the preparation method that open a kind of water dispersibles type alkyl/polyethers amino silicone.
For achieving the above object, the present invention has adopted following technical scheme:
1) ratio that is 1:1.0-1.5 in Si-H key in Silicon Containing Hydrogen resin with the mol ratio of thiazolinyl (C=C) in the raw material that contains thiazolinyl with the raw material that contains thiazolinyl by Silicon Containing Hydrogen resin is directly mixed or mixes in solvent, then carry out hydrosilylation addition reaction and make alkyl/epoxy group(ing) silicone resin intermediate, the described raw material that contains thiazolinyl is made up of small molecules thiazolinyl epoxy compounds and alpha-olefin, and the mol ratio of small molecules thiazolinyl epoxy compounds and alpha-olefin is 4-10:1;
2) alkyl/epoxy group(ing) silicone resin intermediate is mixed in the ratio that in alkyl/epoxy group(ing) silicone resin intermediate, epoxy group(ing) is 1:1-1.2 with the mol ratio of polyetheramine with polyetheramine, then carry out ammonia solution ring-opening reaction and obtain alkyl/polyethers amino silicone.
Described Silicon Containing Hydrogen resin is the siloxane polymer that contains Si-H key and trifunctional Si-O key in structure and be topological framework (as structures such as dendroid, netted, cage shapes).
Described Silicon Containing Hydrogen resin is methyl Silicon Containing Hydrogen resin, phenyl Silicon Containing Hydrogen resin, aminomethyl phenyl Silicon Containing Hydrogen resin or hydrogeneous MQ silicone resin, as 0.1-0.8%, viscosity is 100-6000mPas to the Si-H linkage content of Silicon Containing Hydrogen resin (mole number taking contained Si-H key in every 100g silicone resin represents).
Described small molecules thiazolinyl epoxy compounds is glycidyl allyl ether, glycidyl acrylate or glycidyl methacrylate.
Described alpha-olefin is for containing C
8-18alpha-carbon alkene, as α-octene, α-dodecylene, α-cetene or α-vaccenic acid etc.
Described solvent is the mixture of any one and toluene in alcohol, alcohol ether or ether-ether (mainly comprising Virahol, the trimethyl carbinol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, dihydroxypropane single-ether, propylene glycol monobutyl ether or 1-Methoxy-2-propyl acetate etc.), solvent load is the 0-200% of Silicon Containing Hydrogen resin quality, and the mass ratio of alcohol, alcohol ether or ether-ether and toluene is 1:1-2.
Described hydrosilylation addition reaction is stirring and N
2under protection, carry out, temperature of reaction is 70-100 DEG C, and the reaction times is 0.5-6h; the catalyzer that described hydrosilylation addition reaction adopts is Platinic chloride, 1, and 3-divinyl tetramethyl disiloxane is closed platinum complex, 1,3-dimethyl-1; 3-phenylbenzene-1; 3-divinylsiloxanes is closed platinum complex or 1,3,5; 7-tetramethyl--1; 3,5,7-tetrem thiazolinyl cyclotetrasiloxane closes platinum complex.
Described alkyl/epoxy group(ing) silicone resin intermediate is in molecular structure, to be connected with C simultaneously
8-18alkyl and epoxy group(ing), and structure is the siloxane polymer of the topological frameworks such as netted, dendroid.
Described polyetheramine is that end group is connected with primary amino and mid-block and has the one in the diamine of polyoxyethylene poly-oxygen propylene aether group, the molecular-weight average of polyetheramine is 230-1000, mainly comprise polyetheramine D230, D400, ED-600, ED-900 etc., can directly buy from Huntsman company of the U.S. or Yangzhou Chen Hua Group Co.,Ltd.
The temperature of reaction of described ammonia solution ring-opening reaction is 45-120 DEG C, and the reaction times is 1-4h, and reaction finishes rear steaming except unreacted low-boiling-point substance and solvent.
Described alkyl/polyethers amino silicone is in molecular structure, to be connected with C simultaneously
8-18alkyl and polyethers amino group and structure are the siloxane polymer of the topological frameworks such as netted or dendroid.
Beneficial effect of the present invention is embodied in:
Silicon Containing Hydrogen resin and small molecules thiazolinyl epoxy compounds, alpha-olefin are first carried out hydrosilylation addition reaction synthesis of alkyl/epoxy group(ing) silicone resin intermediate by the present invention, then, again intermediate and polyetheramine are carried out to ammonia solution ring-opening reaction synthesis of alkyl/polyethers amino silicone at 45-120 DEG C, polyethers amino group is introduced in silicone resin structure, can not only improve water-soluble, automatic emulsifying performance and the ionic of silicone resin, and can make the range of application of silicone resin be extended to water-based system as fields such as organic silicone finishing agent, water-borne coatings and coatings.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but the present invention never only limits to these embodiment.
Embodiment 1
To being equipped with, in the there-necked flask of thermometer, reflux condensing tube and electric mixer, to add successively 30g viscosity be methyl Silicon Containing Hydrogen resin (containing Si-H key 0.06mol), 5.7g (0.05mol) glycidyl allyl ether and 1.14g (0.01mol) α-octene that 2080mPas, Si-H linkage content are 0.2%, then stirring and logical N
2under protection, be heated to 70 DEG C; in there-necked flask, add 20ppm catalyzer Platinic chloride insulation reaction 6h again; after reaction, be down to room temperature and obtain the about 36.84g colourless transparent liquid of total amount; be intermediate octyl group/2; 3-epoxypropoxy silicone resin (being called for short octyl group/epoxy group(ing) silicone resin), containing the about 0.05mol of epoxy group(ing).
In intermediate, continue to add 13.8g(0.06mol) polyetheramine D230, after stirring and evenly mixing, reheat and be warming up to 120 DEG C of reaction 1h.After reaction finishes, be that 600mmHg, temperature are to remove unreacted low-boiling-point substance under reduced pressure under 80 DEG C of conditions in gauge pressure, obtain the sticky shape of water white transparency or omit troubled liquor, i.e. octyl group/polyethers amino silicone-230, content approximately 100%.
Embodiment 2
To being equipped with, in the there-necked flask of thermometer, reflux condensing tube and electric mixer, to add successively 30g viscosity be methyl Silicon Containing Hydrogen resin (containing Si-H key 0.03mol), 4.62g (0.0405mol) glycidyl allyl ether and 0.76g (0.0045mol) α-dodecylene that 5900mPas, Si-H linkage content are 0.1%, then stirring and logical N
2under protection, be heated to 100 DEG C; in there-necked flask, add 50ppm catalyzer Platinic chloride insulation reaction 0.5h again; then be that 500mmHg, temperature are 100 DEG C and remove excessive glycidyl allyl ether under reduced pressure in gauge pressure; be down to room temperature and obtain the water white transparency thick liquid of the about 33.67g of total amount; be intermediate dodecyl/epoxy group(ing) silicone resin, containing the about 0.0255mol of epoxy group(ing).
In intermediate, continue to add 7.04g(0.0306mol) polyetheramine D230, stirring and evenly mixing post-heating is warming up to 45 DEG C of reaction 4h.After reaction finishes, be that 600mmHg, temperature are to remove unreacted low-boiling-point substance under reduced pressure under 80 DEG C of conditions in gauge pressure, obtain water white transparency shape thick liquid, i.e. dodecyl/polyethers amino silicone-230, content approximately 100%.
Embodiment 3
To being equipped with, in the there-necked flask of thermometer, reflux condensing tube and electric mixer, to add successively 30g viscosity be hydrogeneous MQ silicone resin (containing Si-H key 0.24mol), 22.98g (0.2016mol) glycidyl allyl ether, 12.7g (0.0504mol) α-vaccenic acid and the 60g Virahol-toluene Mixed Solvent (Virahol: the mass ratio=1:1 of toluene) that 130mPas, Si-H linkage content are 0.8%, then stirring and logical N
2under protection, be heated to 80 DEG C; in there-necked flask, add 20ppm catalyzer 1 again; 3-divinyl tetramethyl disiloxane is closed platinum complex insulation reaction 3h; after reaction, be down to room temperature and obtain the water white transparency thick liquid of the about 125.68g of total amount; be the solution of intermediate octadecyl/epoxy group(ing) silicone resin, containing the about 0.2016mol of epoxy group(ing).
Add 80.64g(0.2016mol to the solution for continuous of intermediate) polyetheramine D400, stirring and evenly mixing post-heating is warming up to 60 DEG C of reaction 2h.Reaction finishes, and reclaims Virahol, and then be that 600mmHg, temperature are under 90 DEG C of conditions, to remove toluene and other low-boiling-point substances under reduced pressure in gauge pressure at 85 DEG C of first normal pressures, obtains translucent thick liquid, i.e. octadecyl/polyethers amino silicone-400, content approximately 100%.
Embodiment 4
To being equipped with, in the there-necked flask of thermometer, reflux condensing tube and electric mixer, to add successively 20g viscosity be aminomethyl phenyl Silicon Containing Hydrogen resin (containing Si-H key 0.06mol), 7.68g (0.054mol) glycidyl methacrylate, 0.68g (0.006mol) α-octene and the 30g propylene glycol monomethyl ether-toluene Mixed Solvent (propylene glycol monomethyl ether: the mass ratio=1:2 of toluene) that 3600mPas, Si-H linkage content are 0.3%, then stirring and logical N
2under protection, be heated to 85 DEG C; in there-necked flask, add 25ppm catalyzer 1 again; 3-dimethyl-1; 3-phenylbenzene-1; 3-divinylsiloxanes is closed platinum complex insulation reaction 2h; after reaction, be down to room temperature and obtain the water white transparency thick liquid of the about 58.36g of total amount, i.e. the solution of intermediate octyl group/epoxy group(ing) silicone resin, containing the about 0.054mol of epoxy group(ing).
Solution for continuous to intermediate adds 34.0g(0.0567mol) polyetheramine ED-600, stirring and evenly mixing post-heating is warming up to 80 DEG C of reaction 3h.Reaction finishes, and is that 600mmHg, temperature are under 100-120 DEG C of condition, to remove toluene and propylene glycol monomethyl ether and low-boiling-point substance under reduced pressure in gauge pressure, obtains the muddy thick liquid of water white transparency-Lve, i.e. octyl group/polyethers amino silicone-600, content approximately 100%.
Embodiment 5
To being equipped with, in the there-necked flask of thermometer, reflux condensing tube and electric mixer, to add successively 10g viscosity be aminomethyl phenyl Silicon Containing Hydrogen resin (containing Si-H key 0.05mol), 5.23g (0.0459mol) glycidyl allyl ether, 1.14g (0.005mol) α-cetene and the 20g 1-Methoxy-2-propyl acetate-toluene Mixed Solvent (1-Methoxy-2-propyl acetate: the mass ratio=1:1 of toluene) that 1060mPas, Si-H linkage content are 0.5%, then stirring and logical N
2under protection, be heated to 85 DEG C; in there-necked flask, add 15ppm catalyzer 1 again; 3-dimethyl-1; 3-phenylbenzene-1-3-divinylsiloxanes is closed platinum complex insulation reaction 1.5h; after reaction, be down to room temperature and obtain the water white transparency thick liquid of the about 36.37g of total amount; be the solution of intermediate hexadecyl/epoxy group(ing) silicone resin, the about 16.37g of epoxy silicone content, containing the about 0.0459mol of epoxy group(ing).
Solution for continuous to intermediate adds 41.9g(0.0459mol) polyetheramine ED-900, stirring and evenly mixing post-heating is warming up to 110 DEG C of reaction 4h.After reaction finishes, be that 600mmHg, temperature are to remove solvent and low-boiling-point substance under reduced pressure under 100-120 DEG C of condition in gauge pressure, obtain water white transparency-translucent thick liquid, i.e. hexadecyl/polyethers amino silicone-900, content approximately 100%.
Get alkyl/polyethers amino silicone spent glycol butyl ether prepared by embodiment 1-5 and be diluted to 50%, with acetic acid tune, pH is about 6, then add water and use dispersion machine emulsification, make solid content and be 15% silicon breast, place after one day, evaluate silicon breast outward appearance with appearance method, the centrifugal 15min of the whizzer that is 3000r/m with rotating speed evaluates the relative stability of silicon breast, and reference is the Silicon Containing Hydrogen resin (oil soluble) of non-modified in embodiment 1-5.Experimental result is in table 1.
The easy emulsifying property of table 1 alkyl/polyethers amino silicone and the performance of relevant emulsion
* centrifugal stability: 3000r/m × 15min
As can be seen from Table 1, chain alkyl/polyethers amino silicone prepared by embodiment of the present invention 1-5 is water-soluble good, centrifugal the having good stability of silicon breast made from it under butyl glycol ether exists, and the Silicon Containing Hydrogen resin of non-modified, insoluble in water, it is dispensed into the emulsion of making in water by force unstable, very easily layering floating oil.Visible, alkyl/polyethers amino silicone prepared by the present invention has water-dispersible really.
Claims (10)
1. water dispersibles a preparation method for type alkyl/polyethers amino silicone, it is characterized in that: comprise the following steps:
1) ratio that is 1:1.0-1.5 in Si-H key with the mol ratio of thiazolinyl with the raw material that contains thiazolinyl by Silicon Containing Hydrogen resin is directly mixed or mixes in solvent, then carry out hydrosilylation addition reaction and make alkyl/epoxy group(ing) silicone resin intermediate, the described raw material that contains thiazolinyl is made up of small molecules thiazolinyl epoxy compounds and alpha-olefin, and the mol ratio of small molecules thiazolinyl epoxy compounds and alpha-olefin is 4-10:1;
2) alkyl/epoxy group(ing) silicone resin intermediate is mixed in the ratio that in alkyl/epoxy group(ing) silicone resin intermediate, epoxy group(ing) is 1:1-1.2 with the mol ratio of polyetheramine with polyetheramine, then carry out ammonia solution ring-opening reaction and obtain alkyl/polyethers amino silicone.
2. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: described Silicon Containing Hydrogen resin is the siloxane polymer that contains Si-H key and trifunctional Si-O key in structure and be topological framework.
3. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: described Silicon Containing Hydrogen resin is methyl Silicon Containing Hydrogen resin, phenyl Silicon Containing Hydrogen resin, aminomethyl phenyl Silicon Containing Hydrogen resin or hydrogeneous MQ silicone resin, the Si-H linkage content of Silicon Containing Hydrogen resin is 0.1-0.8%, and viscosity is 100-6000mPas.
4. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: described small molecules thiazolinyl epoxy compounds is glycidyl allyl ether, glycidyl acrylate or glycidyl methacrylate.
5. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: described alpha-olefin is for containing C
8-18alpha-carbon alkene.
6. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: described solvent is the mixture of any one and toluene in alcohol, alcohol ether or ether-ether, solvent load is the 0-200% of Silicon Containing Hydrogen resin quality, and the mass ratio of alcohol, alcohol ether or ether-ether and toluene is 1:1-2.
7. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: described hydrosilylation addition reaction is stirring and N
2under protection, carry out, temperature of reaction is 70-100 DEG C, and the reaction times is 0.5-6h; the catalyzer that described hydrosilylation addition reaction adopts is Platinic chloride, 1, and 3-divinyl tetramethyl disiloxane is closed platinum complex, 1,3-dimethyl-1; 3-phenylbenzene-1; 3-divinylsiloxanes is closed platinum complex or 1,3,5; 7-tetramethyl--1; 3,5,7-tetrem thiazolinyl cyclotetrasiloxane closes platinum complex.
8. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: described polyetheramine is that end group is connected with primary amino and mid-block and has the one in the diamine of polyoxyethylene poly-oxygen propylene aether group, and the molecular-weight average of polyetheramine is 230-1000.
9. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: the temperature of reaction of described ammonia solution ring-opening reaction is 45-120 DEG C, and the reaction times is 1-4h.
10. a kind of water dispersibles the preparation method of type alkyl/polyethers amino silicone according to claim 1, it is characterized in that: described alkyl/polyethers amino silicone is in molecular structure, to be connected with C simultaneously
8-18alkyl and polyethers amino group and be the siloxane polymer of topological framework.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104262633A (en) * | 2014-09-28 | 2015-01-07 | 烟台德邦先进硅材料有限公司 | Modified MQ resin and synthesis method thereof |
| CN105694062A (en) * | 2016-02-06 | 2016-06-22 | 陕西科技大学 | Cross-linked structure dendritic amino silicone oil and preparation method thereof |
| CN105694046A (en) * | 2016-02-06 | 2016-06-22 | 浙江汉邦化工有限公司 | Preparation method of highly-branched block polyether-aminosiloxane finishing agent |
| CN104262633B (en) * | 2014-09-28 | 2017-01-04 | 烟台德邦先进硅材料有限公司 | A kind of modified MQ resin and synthetic method thereof |
| CN107163254A (en) * | 2017-07-03 | 2017-09-15 | 陕西科技大学 | A kind of preparation method and applications of solvent-borne type hydro-oleophobicity fluorohydrocarbon base silicones |
| CN107540843A (en) * | 2017-08-31 | 2018-01-05 | 华南理工大学 | The function additive of side base containing chain alkyl and epoxy based polysiloxane and preparation method thereof |
| CN109096500A (en) * | 2018-07-06 | 2018-12-28 | 福建拓烯新材料科技有限公司 | A kind of organic siliconresin microemulsion and preparation method |
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| CN104262633A (en) * | 2014-09-28 | 2015-01-07 | 烟台德邦先进硅材料有限公司 | Modified MQ resin and synthesis method thereof |
| CN104262633B (en) * | 2014-09-28 | 2017-01-04 | 烟台德邦先进硅材料有限公司 | A kind of modified MQ resin and synthetic method thereof |
| CN105694062A (en) * | 2016-02-06 | 2016-06-22 | 陕西科技大学 | Cross-linked structure dendritic amino silicone oil and preparation method thereof |
| CN105694046A (en) * | 2016-02-06 | 2016-06-22 | 浙江汉邦化工有限公司 | Preparation method of highly-branched block polyether-aminosiloxane finishing agent |
| CN107163254A (en) * | 2017-07-03 | 2017-09-15 | 陕西科技大学 | A kind of preparation method and applications of solvent-borne type hydro-oleophobicity fluorohydrocarbon base silicones |
| CN107163254B (en) * | 2017-07-03 | 2021-01-29 | 陕西科技大学 | Preparation method and application of solvent type hydrophobic and oleophobic fluorocarbon silicone resin |
| CN107540843A (en) * | 2017-08-31 | 2018-01-05 | 华南理工大学 | The function additive of side base containing chain alkyl and epoxy based polysiloxane and preparation method thereof |
| CN107540843B (en) * | 2017-08-31 | 2020-05-22 | 华南理工大学 | Functional assistant with side group containing long-chain alkyl and epoxy polysiloxane and preparation method thereof |
| CN109096500A (en) * | 2018-07-06 | 2018-12-28 | 福建拓烯新材料科技有限公司 | A kind of organic siliconresin microemulsion and preparation method |
| CN109096500B (en) * | 2018-07-06 | 2021-04-13 | 福建拓烯新材料科技有限公司 | Organic silicon resin microemulsion and preparation method thereof |
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