CN102964900A - Emulsion paint thickener and preparation method thereof - Google Patents
Emulsion paint thickener and preparation method thereof Download PDFInfo
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- CN102964900A CN102964900A CN201210488276XA CN201210488276A CN102964900A CN 102964900 A CN102964900 A CN 102964900A CN 201210488276X A CN201210488276X A CN 201210488276XA CN 201210488276 A CN201210488276 A CN 201210488276A CN 102964900 A CN102964900 A CN 102964900A
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- Prior art keywords
- reaction
- emulsion paint
- preparation
- thickening material
- emulsion
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- 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.)
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- 239000000839 emulsion Substances 0.000 title claims abstract description 24
- 239000003973 paint Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002562 thickening agent Substances 0.000 title claims abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 28
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 230000008719 thickening Effects 0.000 claims abstract description 17
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims abstract description 14
- 239000005058 Isophorone diisocyanate Substances 0.000 claims abstract description 14
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims abstract description 14
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000178 monomer Substances 0.000 claims abstract description 9
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 5
- 238000010792 warming Methods 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 15
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- -1 polyoxyethylene Polymers 0.000 claims description 8
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims description 6
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 claims description 6
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- 239000000080 wetting agent Substances 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- 239000002202 Polyethylene glycol Substances 0.000 abstract 4
- 239000012975 dibutyltin dilaurate Substances 0.000 abstract 1
- 125000001165 hydrophobic group Chemical group 0.000 abstract 1
- 0 *C(**1)C1(C1)[C@]2C1C2*CN=C Chemical compound *C(**1)C1(C1)[C@]2C1C2*CN=C 0.000 description 3
- 239000008118 PEG 6000 Substances 0.000 description 2
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- HGCIXCUEYOPUTN-UHFFFAOYSA-N C1CC=CCC1 Chemical compound C1CC=CCC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 description 1
- VCWNHOPGKQCXIQ-UHFFFAOYSA-N CC1C(C)C(C)CC1 Chemical compound CC1C(C)C(C)CC1 VCWNHOPGKQCXIQ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Landscapes
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to an emulsion paint thickener. The structural formula is as follows: the monomer before an IPDI (isophorone diisocyanate) reaction is isophorone diisocyanate; the monomer before a PEG (polyethylene glycol) reaction is polyethylene glycol; and the monomer before an HDI (Hexamethylene Diisocyanate) reaction is hexamethylene diisocyanate. The preparation method comprises the following steps: under the protection of the nitrogen, mixing polyethylene glycol, hexamethylene diisocyanate, dibutyltin dilaurate with anhydrous acetone, carrying out a backflow reaction, removing the acetone, adding isophorone diisocyanate, octadecanol and toluene, and carrying out a warming reaction to prepare the emulsion paint thickener. Non-specific association can be generated between a hydrophobic group on a thickener branched chain and components such as a wetting agent and an active agent in the emulsion paint, a three-dimensional reticulated structure is formed for thickening, the emulsion paint thickener has higher dragging viscosity, the thickness of the coating can be increased, and the leveling property of a paint film is better; and besides, the hard segment structure of a polymer molecule is increased by adopting a hydrophobic segment on the main chain, the viscosity of the emulsion at high shear is enhanced, emulsion particles can be dispersed easily, and the system is more stable.
Description
Technical field
The invention belongs to the thickening material technical field, be specifically related to a kind of emulsion paint thickening material and preparation method thereof.
Background technology
Thickening material is a kind of key ingredient of emulsion paint, and being affects the most important factor of its rheological property.At present, one of emulsion paint thickening material that hydroxylated cellulose is commonly used, the water-soluble polymer that it is a kind of better performances, range of application is wider, water-soluble after, give birth to strong hydration with steeping in water for reconstitution, produce between molecular chain and twine, thereby increased solution viscosity.But a little less than the cellulosic molecule absorption, as easy as rolling off a logly replaced by wetting agent, the tensio-active agent in the emulsion in the lacquer etc., be free on aqueous phase, thereby flocculation appears, and because the Mierocrystalline cellulose relative molecular weight is usually very high, cause coating viscosity under high shear rate little, fullness ratio and levelling property that impact is filmed.
Summary of the invention
The technical problem that the present invention mainly solves is: a kind of polyether(poly)urethane association emulsion paint thickening material is provided.
The technical scheme that mainly provides of the present invention: a kind of emulsion paint thickening material, its structural formula is:
Wherein, monomer is isophorone diisocyanate before the IPDI reaction; Monomer is polyoxyethylene glycol before the PEG reaction; Monomer is hexamethylene diisocyanate before the HDI reaction.
Second technical problem to be solved by this invention is: the preparation method that a kind of emulsion paint thickening material is provided.
For solving second technical problem, technical scheme provided by the invention is: a kind of preparation method of emulsion paint thickening material the steps include:
Under nitrogen protection; polyoxyethylene glycol and hexamethylene diisocyanate are added reactor; add dibutyl tin laurate, anhydrous propanone; be heated to 55-65 ℃, back flow reaction 5-6h, when the content of isocyanate group behind certain value; acetone is removed in underpressure distillation; add isophorone diisocyanate, stearyl alcohol, toluene, be warming up to 120-135 ℃ of reaction 2-3h, namely make the polyether(poly)urethane associative thickener.
The molar ratio of described polyoxyethylene glycol, hexamethylene diisocyanate, dibutyl tin laurate, anhydrous propanone, isophorone diisocyanate, stearyl alcohol, toluene is 1.5-2.0:1:0.2-0.3:10-20:1.2-1.8:2.0-3.0:10-15.
Described isocyanate group detection method is the Di-n-Butyl Amine method, when volumetric molar concentration reaches 0.4-0.7mol/L, reacts and finishes.
The number-average molecular weight of described polyoxyethylene glycol is 10000 ~ 10500.
Beneficial effect of the present invention is: the hydrophobic grouping on this thickening material side chain can and emulsion paint in the components such as wetting agent, promoting agent between produce nonspecific association, form simultaneously tridimensional network and thickening, have higher dragging and shoot a retrievable arrow viscosity, be conducive to increase the thickness of coating, the levelling property of paint film is better; Hydrophobic section on the main chain has increased the polymer molecule hard segment structure, improves the viscosity under the emulsion high-shear, help emulsion particle dispersion, make system more stable.
Embodiment
Be described in further detail in conjunction with specific embodiments, make advantage of the present invention more obvious.Should be appreciated that content wherein is just with explaining, and absolutely not protection scope of the present invention is construed as limiting.The experimental technique of unreceipted actual conditions in the following example usually according to normal condition, or carries out according to the condition that manufacturer advises.
Embodiment 1
Under nitrogen protection; 10mol PEG-6000 0 and 6mol hexamethylene diisocyanate are dropped into reactor; add the 1.2mol dibutyl tin laurate; add the 120mol anhydrous propanone; be heated to 55-60 ℃, back flow reaction 5-6h, when the content of isocyanate group behind 0.48-0.52mol/L; revolve steaming, remove acetone.Add 8.0mol isophorone diisocyanate, 12mol stearyl alcohol, 62mol toluene, be warming up to 120-135 ℃ of reaction 2-3h, namely make the polyether(poly)urethane associative thickener.
Embodiment 2
Under nitrogen protection; 18mol PEG-6000 0 and 10mol hexamethylene diisocyanate are dropped into reactor; add the 2mol dibutyl tin laurate; add the 150mol anhydrous propanone; be heated to 55-65 ℃, back flow reaction 5-6h is after the content of isocyanate group is 0.65-0.7mol/L; revolve steaming, remove acetone.Add 15mol isophorone diisocyanate, 23mol stearyl alcohol, 110mol toluene, be warming up to 120-135 ℃ of reaction 2-3h, namely make the polyether(poly)urethane associative thickener.
Claims (5)
2. the preparation method of a kind of emulsion paint thickening material claimed in claim 1 the steps include:
Under nitrogen protection; polyoxyethylene glycol and hexamethylene diisocyanate are added reactor; add dibutyl tin laurate, anhydrous propanone; be heated to 55-65 ℃, back flow reaction 5-6h, when the content of isocyanate group behind certain value; acetone is removed in underpressure distillation; add isophorone diisocyanate, stearyl alcohol, toluene, be warming up to 120-135 ℃ of reaction 2-3h, namely make the polyether(poly)urethane associative thickener.
3. the preparation method of a kind of emulsion paint thickening material according to claim 2, it is characterized in that: the molar ratio of described polyoxyethylene glycol, hexamethylene diisocyanate, dibutyl tin laurate, anhydrous propanone, isophorone diisocyanate, stearyl alcohol, toluene is 1.5-2.0:1:0.2-0.3:10-20:1.2-1.8:2.0-3.0:10-15.
4. the preparation method of a kind of emulsion paint thickening material according to claim 3, it is characterized in that: described isocyanate group detection method is the Di-n-Butyl Amine method, when volumetric molar concentration reaches 0.4-0.7mol/L, reaction finishes.
5. the preparation method of any described a kind of emulsion paint thickening material of claim according to claim 2-4, it is characterized in that: the number-average molecular weight of described polyoxyethylene glycol is 10000 ~ 10500.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210488276XA CN102964900A (en) | 2012-11-26 | 2012-11-26 | Emulsion paint thickener and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210488276XA CN102964900A (en) | 2012-11-26 | 2012-11-26 | Emulsion paint thickener and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102964900A true CN102964900A (en) | 2013-03-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210488276XA Pending CN102964900A (en) | 2012-11-26 | 2012-11-26 | Emulsion paint thickener and preparation method thereof |
Country Status (1)
| Country | Link |
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| CN (1) | CN102964900A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982045A (en) * | 2019-11-21 | 2020-04-10 | 万华化学集团股份有限公司 | Low-viscosity and low-color-number isocyanate curing agent, and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5916967A (en) * | 1997-05-02 | 1999-06-29 | Rohm And Haas Company | Mixed surfactant and hydrophobically-modified polymer compositions |
| CN1511895A (en) * | 2002-12-27 | 2004-07-14 | 上海市涂料研究所 | Polyurea polyurethane associated thickening agent for latex paint |
| CN1840587A (en) * | 2005-03-28 | 2006-10-04 | 深圳市海川实业股份有限公司 | Method for preparing aqueous polyurethane thickener |
| CN1840588A (en) * | 2005-03-28 | 2006-10-04 | 深圳市海川实业股份有限公司 | Method for preparing association thickener for latex paint |
-
2012
- 2012-11-26 CN CN201210488276XA patent/CN102964900A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5916967A (en) * | 1997-05-02 | 1999-06-29 | Rohm And Haas Company | Mixed surfactant and hydrophobically-modified polymer compositions |
| CN1511895A (en) * | 2002-12-27 | 2004-07-14 | 上海市涂料研究所 | Polyurea polyurethane associated thickening agent for latex paint |
| CN1840587A (en) * | 2005-03-28 | 2006-10-04 | 深圳市海川实业股份有限公司 | Method for preparing aqueous polyurethane thickener |
| CN1840588A (en) * | 2005-03-28 | 2006-10-04 | 深圳市海川实业股份有限公司 | Method for preparing association thickener for latex paint |
Non-Patent Citations (1)
| Title |
|---|
| 娄光伟: "聚醚型聚氨酯增稠剂的合成与性能研究", 《中国优秀硕士学位论文全文数据库》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110982045A (en) * | 2019-11-21 | 2020-04-10 | 万华化学集团股份有限公司 | Low-viscosity and low-color-number isocyanate curing agent, and preparation method and application thereof |
| CN110982045B (en) * | 2019-11-21 | 2022-01-07 | 万华化学集团股份有限公司 | Low-viscosity and low-color-number isocyanate curing agent, and preparation method and application thereof |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20130313 |