CN104927039B - A kind of silicone alkyd and preparation method thereof - Google Patents
A kind of silicone alkyd and preparation method thereof Download PDFInfo
- Publication number
- CN104927039B CN104927039B CN201510260504.1A CN201510260504A CN104927039B CN 104927039 B CN104927039 B CN 104927039B CN 201510260504 A CN201510260504 A CN 201510260504A CN 104927039 B CN104927039 B CN 104927039B
- Authority
- CN
- China
- Prior art keywords
- parts
- silicone alkyd
- cottonseed oil
- glutaconate
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920000180 alkyd Polymers 0.000 title claims abstract description 38
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 235000012343 cottonseed oil Nutrition 0.000 claims abstract description 28
- 239000002385 cottonseed oil Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- XVOUMQNXTGKGMA-OWOJBTEDSA-N (E)-glutaconic acid Chemical compound OC(=O)C\C=C\C(O)=O XVOUMQNXTGKGMA-OWOJBTEDSA-N 0.000 claims abstract description 23
- 229920000728 polyester Polymers 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000178 monomer Substances 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000010703 silicon Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000010792 warming Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical group CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 4
- HVGYYRCQMTYPPY-UHFFFAOYSA-N methyl-tri(propan-2-yl)silane Chemical compound CC(C)[Si](C)(C(C)C)C(C)C HVGYYRCQMTYPPY-UHFFFAOYSA-N 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 2
- 229920003232 aliphatic polyester Polymers 0.000 claims 1
- 238000004132 cross linking Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000412 dendrimer Substances 0.000 description 2
- 229920000736 dendritic polymer Polymers 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000002320 enamel (paints) Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- QBKSWRVVCFFDOT-UHFFFAOYSA-N gossypol Chemical compound CC(C)C1=C(O)C(O)=C(C=O)C2=C(O)C(C=3C(O)=C4C(C=O)=C(O)C(O)=C(C4=CC=3C)C(C)C)=C(C)C=C21 QBKSWRVVCFFDOT-UHFFFAOYSA-N 0.000 description 2
- 239000003981 vehicle Substances 0.000 description 2
- 230000002087 whitening effect Effects 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 206010043298 Testicular atrophy Diseases 0.000 description 1
- QHOPXUFELLHKAS-UHFFFAOYSA-N Thespesin Natural products CC(C)c1c(O)c(O)c2C(O)Oc3c(c(C)cc1c23)-c1c2OC(O)c3c(O)c(O)c(C(C)C)c(cc1C)c23 QHOPXUFELLHKAS-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229930000755 gossypol Natural products 0.000 description 1
- 229950005277 gossypol Drugs 0.000 description 1
- 229920000587 hyperbranched polymer Polymers 0.000 description 1
- 208000000509 infertility Diseases 0.000 description 1
- 230000036512 infertility Effects 0.000 description 1
- 231100000535 infertility Toxicity 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002991 molded plastic Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Polyesters Or Polycarbonates (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a kind of silicone alkyd, raw material includes by weight：30 40 parts of terminal hydroxy group aliphatic hyper-branched polyester, 20 30 parts of crude cottonseed oil, 50 60 parts of glutaconate solution, 38 parts of dimethylbenzene, 25 30 parts of organic silicon monomer, 10 15 parts of deionized water.The invention also discloses a kind of preparation methods of silicone alkyd.The present invention has excellent filming performance, and activity of cross-linking reaction is high, and curing rate is fast, and viscosity is low, dissolubility is good, also has excellent water resistance, heat resistance and stability.The present invention uses crude cottonseed oil, not only greatly reduces production cost, while solving the process problem of crude cottonseed oil again, energy saving, turns waste into wealth, safety and environmental protection.
Description
Technical field
The present invention relates to alkyd resin technical field more particularly to a kind of silicone alkyd and its preparation sides
Method.
Background technology
Alkyd resin is mainly used for paint, coating, is widely used in metal protection, furniture, vehicle, building etc.,
It also is used as the insulating layer of enameled wire, ink is made and is widely used in printing industry, is also used for manufacture moulded plastic in addition.Alkyd
Resin is the main film forming substance of traditional mixed paint, enamel paint etc., has the characteristics that good weatherability, adhesive force are good and bright, plentiful,
And it is easy for construction, dry or drying enamel paint, priming paint, finishing coat and the varnish of a variety of different performances can be made into other resins, extensively
For the applications such as the buildings such as bridge and machinery, vehicle, ship, aircraft, instrument.
Present living standard greatly improves, and people often do not use cottonseed oil, and contain gossypol, glue in crude cotton oil
Matter and wax, inferior quality should not directly be eaten, and refinery practice is also complex, and refining cost is high.And eat crude cottonseed
Oil can cause androgone to damage, and lead to orchiatrophy, and be generated without sperm, cause infertility.Present crude cottonseed oil often by
It is discarded.
Invention content
Technical problems based on background technology, the present invention propose a kind of silicone alkyd and its preparation
Method has excellent filming performance, and activity of cross-linking reaction is high, and curing rate is fast, and viscosity is low, dissolubility is good, also has
Excellent water resistance, heat resistance and stability.
A kind of silicone alkyd proposed by the present invention, raw material include by weight：Terminal hydroxy group aliphatic is super
30-40 parts of branched polyester, crude cottonseed oil 20-30 parts, 50-60 parts of glutaconate solution, 3-8 parts of dimethylbenzene, organic silicon monomer
25-30 parts, 10-15 parts of deionized water.
In specific embodiment, the parts by weight of terminal hydroxy group aliphatic hyper-branched polyester can be 30 parts, 31 parts, 32 parts, 33 parts,
34 parts, 35 parts, 36 parts, 37 parts, 38 parts, 39 parts, 40 parts, the parts by weight of crude cottonseed oil can be 20 parts, 21 parts, 22 parts, 23
Part, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, the parts by weight of glutaconate solution can be 50 parts, 51 parts, 52
Part, 53 parts, 54 parts, 55 parts, 56 parts, 57 parts, 58 parts, 59 parts, 60 parts, the parts by weight of dimethylbenzene can be 3 parts, 4 parts, 5 parts, 6
Part, 7 parts, 8 parts, the parts by weight of organic silicon monomer can be 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, the weight of deionized water
It can be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts to measure part.
Preferably, organic silicon monomer is vinyltriethoxysilane, methyltriethoxysilane, methyl triisopropyl silicon
One kind in alkane.
Preferably, terminal hydroxy group aliphatic hyper-branched polyester, crude cottonseed oil, glutaconate solution weight ratio be 33-37：
22-28：54-56.
Preferably, the mass fraction of glutaconate solution is 40-55wt%.
Preferably, raw material includes by weight：33-37 parts of terminal hydroxy group aliphatic hyper-branched polyester, crude cottonseed oil 22-
28 parts, 54-56 parts of glutaconate solution, 5-6 parts of dimethylbenzene, 27-28 parts of organic silicon monomer, 12-14 parts of deionized water.
The preparation method for the above-mentioned silicone alkyd that the present invention also proposes, includes the following steps：
S1, it is filled with oxygen volume content≤2% in nitrogen to reaction kettle into reaction kettle, it is super adds terminal hydroxy group aliphatic
Branched polyester, crude cottonseed oil, glutaconate solution are warming up to 200-220 DEG C, keep the temperature 2-4h, in heating and insulating process not
Stop stirring；
S2,170-190 DEG C is cooled to again, after dimethylbenzene is added, 210-245 DEG C of reflux water-dividing 3-4h is warming up to, until resin
Acid value≤8mg/g, stirring is cooled to 45-55 DEG C and obtains mixed material；
S3, mixed material is warming up to 120-140 DEG C, organic silicon monomer is added, deionized water is then added dropwise, keep the temperature 2.5-
2.8h is down to room temperature, and silicone alkyd is obtained by filtration.
Preferably, in S1, heating rate is 8-10 DEG C/min.
Preferably, in S3, deionized water drop rate is 2-5ml/min.
Dissaving polymer (Hyperbranched Polymer, HBP) has unique physical and chemical properties, is close
One of the hot spot that polymeric material field is studied over year.Compared with linear macromolecule, HBP have special branched molecular structure,
Viscosity of the less entanglement of strand to be not easy to crystallize, under chemical reactivity is high, dissolubility is good and solution or molten condition compared with
Low property；Compared to dendrimer similar in structure, there are more defect in HBP molecules, the degree of branching is low, average molecular
Mass Distribution is wide, and isomers is more, but most of characteristics with dendrimer, and its synthetic method is simple, is not necessarily to cumbersome consumption
When purifying and separation process, cost is greatly reduced, more suitable for large-scale production and application.
Using terminal hydroxy group aliphatic hyper-branched polyester and crude cottonseed oil, glutaconate solution esterification occurs for the present invention
Alkyd resin is generated, is modified to obtain silicone alkyd further through grafted-organosilicon.Due to terminal hydroxy group aliphatic
Hyper-branched polyester has the branched structure of height, makes the intermolecular less chain entanglement of the present invention, is not easy to crystallize, so as to excellent
Different filming performance, and terminal hydroxy group aliphatic hyper-branched polyester coordinates with crude cottonseed oil, glutaconate solution, can increase this
While invention activity of cross-linking reaction, its system viscosity is reduced, and plays the role of accelerating dried coating film process, and it has
Low-viscosity and highly dissoluble can reduce the usage amount of organic solvent, improve mobility of the present invention；Crude cottonseed oil is used simultaneously,
Production cost is not only greatly reduced, while solving the process problem of crude cottonseed oil again, it is energy saving, turn waste into wealth, pacifies
Loopful is protected；And after organosilicon grafting, make the present invention that there is excellent water resistance and heat resistance, improves the stability of product；It prepares
Heating rate is limited in the process as 8-10 DEG C/min, fat polymerization reaction is made efficiently to carry out, and limits deionized water drop rate
For 2-5ml/min, the generation of organosilicon self-polymeric reaction was not only avoided, but also improve production efficiency.
In conclusion the present invention has excellent filming performance, activity of cross-linking reaction is high, and curing rate is fast, and viscosity
It is low, dissolubility is good, also have excellent water resistance, heat resistance and stability.
Description of the drawings
Fig. 1 is a kind of flow diagram of the preparation method of silicone alkyd proposed by the present invention.
Specific implementation mode
As shown in FIG. 1, FIG. 1 is a kind of flow signals of the preparation method of silicone alkyd proposed by the present invention
Figure.
Referring to Fig.1, the preparation method of above-mentioned silicone alkyd proposed by the present invention, includes the following steps：
S1, it is filled with oxygen volume content≤2% in nitrogen to reaction kettle into reaction kettle, it is super adds terminal hydroxy group aliphatic
Branched polyester, crude cottonseed oil, glutaconate solution are warming up to 200-220 DEG C, keep the temperature 2-4h, in heating and insulating process not
Stop stirring；
S2,170-190 DEG C is cooled to again, after dimethylbenzene is added, 210-245 DEG C of reflux water-dividing 3-4h is warming up to, until resin
Acid value≤8mg/g, stirring is cooled to 45-55 DEG C and obtains mixed material；
S3, mixed material is warming up to 120-140 DEG C, organic silicon monomer is added, deionized water is then added dropwise, keep the temperature 2.5-
2.8h is down to room temperature, and silicone alkyd is obtained by filtration.
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of silicone alkyd proposed by the present invention, raw material include by weight：Terminal hydroxy group aliphatic is super
30 parts of branched polyester, 30 parts of crude cottonseed oil, 50 parts of glutaconate solution, 8 parts of dimethylbenzene, vinyltriethoxysilane 25
Part, 15 parts of deionized water.
The preparation method for the above-mentioned silicone alkyd that the present invention also proposes, includes the following steps：
S1, it is filled with oxygen volume content≤2% in nitrogen to reaction kettle into reaction kettle, it is super adds terminal hydroxy group aliphatic
Branched polyester, crude cottonseed oil, glutaconate solution are warming up to 210 DEG C, and heating rate is 10 DEG C/min, keeps the temperature 3.2h, heating
It is kept stirring in insulating process；
S2,175 DEG C are cooled to again, after dimethylbenzene is added, be warming up to 235 DEG C of reflux water-dividing 3.4h, until the acid value of resin≤
8mg/g, stirring are cooled to 53 DEG C and obtain mixed material；
S3, mixed material is warming up to 125 DEG C, vinyltriethoxysilane is added, deionized water is then added dropwise, kept the temperature
2.7h is down to room temperature, and silicone alkyd is obtained by filtration.
Embodiment 2
A kind of silicone alkyd proposed by the present invention, raw material include by weight：Terminal hydroxy group aliphatic is super
37 parts of branched polyester, 22 parts of crude cottonseed oil, 56 parts of glutaconate solution, 5 parts of dimethylbenzene, 28 parts of methyltriethoxysilane,
12 parts of deionized water.
The preparation method for the above-mentioned silicone alkyd that the present invention also proposes, includes the following steps：
S1, it is filled with oxygen volume content≤2% in nitrogen to reaction kettle into reaction kettle, it is super adds terminal hydroxy group aliphatic
Branched polyester, crude cottonseed oil, glutaconate solution, are warming up to 200 DEG C, and heating rate is 8 DEG C/min, keep the temperature 4h, heating and
It is kept stirring in insulating process；
S2,170 DEG C are cooled to again, after dimethylbenzene is added, be warming up to 245 DEG C of reflux water-dividing 3h, until the acid value of resin≤
8mg/g, stirring are cooled to 55 DEG C and obtain mixed material；
S3, mixed material is warming up to 120 DEG C, methyltriethoxysilane is added, deionized water is then added dropwise, speed is added dropwise
Rate is 3ml/min, keeps the temperature 2.8h, is down to room temperature, silicone alkyd is obtained by filtration.
Embodiment 3
A kind of silicone alkyd proposed by the present invention, raw material include by weight：Terminal hydroxy group aliphatic is super
33 parts of branched polyester, 28 parts of crude cottonseed oil, 54 parts of glutaconate solution, 6 parts of dimethylbenzene, 27 parts of methyl tri isopropyl silane,
14 parts of deionized water.
The preparation method for the above-mentioned silicone alkyd that the present invention also proposes, includes the following steps：
S1, it is filled with oxygen volume content≤2% in nitrogen to reaction kettle into reaction kettle, it is super adds terminal hydroxy group aliphatic
Branched polyester, crude cottonseed oil, glutaconate solution, are warming up to 220 DEG C, and heating rate is 9 DEG C/min, keep the temperature 2h, heating and
It is kept stirring in insulating process；
S2,190 DEG C are cooled to again, after dimethylbenzene is added, be warming up to 210 DEG C of reflux water-dividing 4h, until the acid value of resin≤
8mg/g, stirring are cooled to 45 DEG C and obtain mixed material；
S3, mixed material is warming up to 140 DEG C, methyl tri isopropyl silane is added, deionized water is then added dropwise, speed is added dropwise
Rate is 5ml/min, keeps the temperature 2.5h, is down to room temperature, silicone alkyd is obtained by filtration.
Embodiment 4
A kind of silicone alkyd proposed by the present invention, raw material include by weight：Terminal hydroxy group aliphatic is super
40 parts of branched polyester, 20 parts of crude cottonseed oil, 60 parts of glutaconate solution, 3 parts of dimethylbenzene, 30 parts of methyltriethoxysilane,
10 parts of deionized water.
The preparation method for the above-mentioned silicone alkyd that the present invention also proposes, includes the following steps：
S1, it is filled with oxygen volume content≤2% in nitrogen to reaction kettle into reaction kettle, it is super adds terminal hydroxy group aliphatic
Branched polyester, crude cottonseed oil, glutaconate solution are warming up to 215 DEG C, keep the temperature 3h, are kept stirring in heating and insulating process；
S2,180 DEG C are cooled to again, after dimethylbenzene is added, be warming up to 220 DEG C of reflux water-dividing 3.6h, until the acid value of resin≤
8mg/g, stirring are cooled to 48 DEG C and obtain mixed material；
S3, mixed material is warming up to 130 DEG C, methyltriethoxysilane is added, deionized water is then added dropwise, speed is added dropwise
Rate is 2ml/min, keeps the temperature 2.6h, is down to room temperature, silicone alkyd is obtained by filtration.
Using 1-4 of the embodiment of the present invention as experimental group, as a control group using common alkyd resin, performance comparison is carried out
Detection, result are as follows：
| Detection project | Control group | Experimental group |
| Content of fatty acid/% | 48 | 48 |
| Viscosity/mPas | 26000 | 4300 |
Performance comparison detection is carried out after experimental group and control group are carried out plane spraying, result is as follows：
| Detection project | Control group | Experimental group |
| Surface drying/h | 2 | 2 |
| Do solid work/h | 45 | 45 |
| 7 days hardness | 2B | 2H |
| Water resistance detects | 36h non-whitenings are not blistering | 72h non-whitenings are not blistering |
| Heat resistance detects (200 DEG C) | 1h is bubbled | It is not bubbled for 24 hours |
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of silicone alkyd, which is characterized in that its raw material is grouped as by following group by weight：Terminal hydroxy group fat
Hyper-branched polyester 30-40 parts of fat race, crude cottonseed oil 20-30 parts, 50-60 parts of glutaconate solution, 3-8 parts of dimethylbenzene is organic
25-30 parts of silicon monomer, 10-15 parts of deionized water；
Organic silicon monomer is vinyltriethoxysilane or methyl tri isopropyl silane；
The preparation method of the silicone alkyd, includes the following steps：
S1, it is filled with oxygen volume content≤2% in nitrogen to reaction kettle into reaction kettle, it is hyperbranched adds terminal hydroxy group aliphatic
Polyester, crude cottonseed oil, glutaconate solution are warming up to 200-220 DEG C, keep the temperature 2-4h, do not stop to stir in heating and insulating process
It mixes；
S2,170-190 DEG C is cooled to again, after dimethylbenzene is added, 210-245 DEG C of reflux water-dividing 3-4h is warming up to, until the acid of resin
Value≤8mg/g, stirring are cooled to 45-55 DEG C and obtain mixed material；
S3, mixed material is warming up to 120-140 DEG C, organic silicon monomer is added, deionized water is then added dropwise, keep the temperature 2.5-
2.8h is down to room temperature, and silicone alkyd is obtained by filtration；
In S3, deionized water drop rate is 2-5ml/min.
2. silicone alkyd according to claim 1, which is characterized in that terminal hydroxy group aliphatic hyper-branched polyester,
Crude cottonseed oil, glutaconate solution weight ratio be 33-37：22-28：54-56.
3. silicone alkyd according to claim 1 or claim 2, which is characterized in that the quality of glutaconate solution point
Number is 40-55wt%.
4. silicone alkyd according to claim 1 or claim 2, which is characterized in that its raw material is by weight by as follows
Group is grouped as：33-37 parts of terminal hydroxy group aliphatic hyper-branched polyester, crude cottonseed oil 22-28 parts, 54-56 parts of glutaconate solution,
5-6 parts of dimethylbenzene, 27-28 parts of organic silicon monomer, 12-14 parts of deionized water.
5. silicone alkyd according to claim 1, which is characterized in that in S1, heating rate be 8-10 DEG C/
min。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510260504.1A CN104927039B (en) | 2015-05-20 | 2015-05-20 | A kind of silicone alkyd and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510260504.1A CN104927039B (en) | 2015-05-20 | 2015-05-20 | A kind of silicone alkyd and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104927039A CN104927039A (en) | 2015-09-23 |
| CN104927039B true CN104927039B (en) | 2018-10-12 |
Family
ID=54114478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510260504.1A Active CN104927039B (en) | 2015-05-20 | 2015-05-20 | A kind of silicone alkyd and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104927039B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992468A (en) * | 2014-05-23 | 2014-08-20 | 三棵树涂料股份有限公司 | Hyperbranch-modified alkyd resin and preparation method thereof |
| CN104086761A (en) * | 2014-06-05 | 2014-10-08 | 华南理工大学 | Aqueous organosilicone-modified alkyd resin and preparing method thereof |
| CN104151537A (en) * | 2014-07-25 | 2014-11-19 | 青岛展辰新材料有限公司 | Low-odor acrylic modified alkyd resin and preparation method thereof |
| CN104448282A (en) * | 2014-12-18 | 2015-03-25 | 江苏柏鹤涂料有限公司 | Alkyd acrylic ester and photocureable coating thereof |
-
2015
- 2015-05-20 CN CN201510260504.1A patent/CN104927039B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992468A (en) * | 2014-05-23 | 2014-08-20 | 三棵树涂料股份有限公司 | Hyperbranch-modified alkyd resin and preparation method thereof |
| CN104086761A (en) * | 2014-06-05 | 2014-10-08 | 华南理工大学 | Aqueous organosilicone-modified alkyd resin and preparing method thereof |
| CN104151537A (en) * | 2014-07-25 | 2014-11-19 | 青岛展辰新材料有限公司 | Low-odor acrylic modified alkyd resin and preparation method thereof |
| CN104448282A (en) * | 2014-12-18 | 2015-03-25 | 江苏柏鹤涂料有限公司 | Alkyd acrylic ester and photocureable coating thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104927039A (en) | 2015-09-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106243273B (en) | A kind of hydroxyl acrylic emulsion and the preparation method and application thereof with core-shell structure | |
| CN104072742A (en) | Epoxy-modified water-based alkyd resin and water-based alkyd amino stoving varnish and preparation method of epoxy-modified water-based alkyd resin and water-based alkyd amino stoving varnish. | |
| CN103881341A (en) | Tung oil derivative-modified unsaturated polyester resin composition and preparation method thereof | |
| CN102702493B (en) | Alkyd resin for matte wood lacquer and preparation method of alkyd resin | |
| CN103540217B (en) | The double-component aqueous car paint of acrylate resin that a kind of aziridine is crosslinked and its preparation method | |
| CN102585700A (en) | Method for preparing UV (ultraviolet)-curable high-temperature-resistant and corrosion-resistant organic silicon/silica hybrid coating | |
| CN105837773A (en) | Preparation method of double-modified hyperbranched waterborne polyurethane emulsion with silicone and renewable vegetable oil | |
| CN107033296A (en) | Extra-weather-proof polysiloxane-modified acrylic resin and finish paint preparation method | |
| CN109593335A (en) | One kind modified water-based alkyd resin of polystyrene microsphere containing carboxyl and preparation method thereof | |
| CN106893087A (en) | A kind of aqueous polyester resin and preparation method thereof | |
| CN104744645A (en) | Preparation method for high-resistance inorganic-organic composite modified acrylic epoxy ester resin | |
| CN104178022A (en) | Preparation method of heat-resistant imporous enameled wire insulating paint for high speed machines | |
| CN104927000B (en) | Styrene modified alkyd resin and preparation method thereof | |
| CN105131698A (en) | Low free TDI (toluene diisocynate) curing agent and preparation method | |
| CN104927039B (en) | A kind of silicone alkyd and preparation method thereof | |
| CN109942803B (en) | Esterified capped allyl polyether and preparation method thereof | |
| CN108546485B (en) | High-solid-content organic-inorganic hybrid resin and preparation method thereof | |
| CN111234640B (en) | Styrene-acrylic emulsion for spraying and quick setting, preparation method and application in waterproof coating | |
| CN100513500C (en) | Self-curing polyurethane insulating varnish and its production | |
| CN109134829B (en) | Anti-tack epoxy curing agent and preparation method and application thereof | |
| CN104311810A (en) | Cheap dicyclopentadiene modified unsaturated polyester resin and preparation method thereof | |
| CN113136013B (en) | Acrylic acid modified vinyl organic silicon resin and preparation method thereof | |
| CN107216427A (en) | A kind of block modified polyurethane/acrylate emulsion of unsaturated polyester resin and preparation method thereof | |
| CN103614059B (en) | A kind of preparation method of water-based tung oil/acrylic resin insulation paint | |
| CN109880070B (en) | Modified water-based polyester resin dispersoid for water-based baking paint and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Organic silicone-modified alkyd resin and preparation method thereof Effective date of registration: 20190618 Granted publication date: 20181012 Pledgee: Tianchang Science and Technology Financing Guarantee Co., Ltd. Pledgor: Anhui Province Jindun Paint Co., Ltd. Registration number: 2019340000309 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20200616 Granted publication date: 20181012 Pledgee: Tianchang Science and Technology Financing Guarantee Co.,Ltd. Pledgor: ANHUI JINDUN PAINT Co.,Ltd. Registration number: 2019340000309 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Organic silicone-modified alkyd resin and preparation method thereof Effective date of registration: 20200616 Granted publication date: 20181012 Pledgee: Tianchang Science and Technology Financing Guarantee Co.,Ltd. Pledgor: ANHUI JINDUN PAINT Co.,Ltd. Registration number: Y2020990000627 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20210329 Granted publication date: 20181012 Pledgee: Tianchang Science and Technology Financing Guarantee Co.,Ltd. Pledgor: ANHUI JINDUN PAINT Co.,Ltd. Registration number: Y2020990000627 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Organic silicon modified alkyd resin and its preparation method Effective date of registration: 20210401 Granted publication date: 20181012 Pledgee: Tianchang Science and Technology Financing Guarantee Co.,Ltd. Pledgor: ANHUI JINDUN PAINT Co.,Ltd. Registration number: Y2021980002363 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220325 Granted publication date: 20181012 Pledgee: Tianchang Science and Technology Financing Guarantee Co.,Ltd. Pledgor: ANHUI JINDUN PAINT Co.,Ltd. Registration number: Y2021980002363 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |