CN106866950B - Interior wall sealing wax aqueous alkide resin emulsion and preparation method thereof - Google Patents
Interior wall sealing wax aqueous alkide resin emulsion and preparation method thereof Download PDFInfo
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- CN106866950B CN106866950B CN201710017411.5A CN201710017411A CN106866950B CN 106866950 B CN106866950 B CN 106866950B CN 201710017411 A CN201710017411 A CN 201710017411A CN 106866950 B CN106866950 B CN 106866950B
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- emulsifier
- acid
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229920005989 resin Polymers 0.000 title claims abstract description 20
- 239000011347 resin Substances 0.000 title claims abstract description 20
- 239000012173 sealing wax Substances 0.000 title claims abstract description 18
- 239000000839 emulsion Substances 0.000 title claims abstract description 17
- 238000004945 emulsification Methods 0.000 title abstract description 4
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 21
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 15
- 150000001450 anions Chemical group 0.000 claims abstract description 10
- 239000012875 nonionic emulsifier Substances 0.000 claims abstract description 9
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims abstract description 9
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims abstract description 9
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims abstract description 7
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229960002887 deanol Drugs 0.000 claims abstract description 5
- 239000012972 dimethylethanolamine Substances 0.000 claims abstract description 5
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims abstract description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 59
- 239000000178 monomer Substances 0.000 claims description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 8
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- -1 sorbierite Chemical compound 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001244 carboxylic acid anhydrides Chemical group 0.000 claims description 4
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 4
- 229920000233 poly(alkylene oxides) Polymers 0.000 claims description 4
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 claims description 3
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 3
- JCTXKRPTIMZBJT-UHFFFAOYSA-N 2,2,4-trimethylpentane-1,3-diol Chemical class CC(C)C(O)C(C)(C)CO JCTXKRPTIMZBJT-UHFFFAOYSA-N 0.000 claims description 2
- BGQUJDPWPVVEGV-UHFFFAOYSA-N 2,2-dimethylhexane-1,3-diol Chemical compound CCCC(O)C(C)(C)CO BGQUJDPWPVVEGV-UHFFFAOYSA-N 0.000 claims description 2
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 claims description 2
- ALQSHHUCVQOPAS-UHFFFAOYSA-N Pentane-1,5-diol Chemical class OCCCCCO ALQSHHUCVQOPAS-UHFFFAOYSA-N 0.000 claims description 2
- BMRWNKZVCUKKSR-UHFFFAOYSA-N butane-1,2-diol Chemical class CCC(O)CO BMRWNKZVCUKKSR-UHFFFAOYSA-N 0.000 claims description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical class OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- SXCBDZAEHILGLM-UHFFFAOYSA-N heptane-1,7-diol Chemical class OCCCCCCCO SXCBDZAEHILGLM-UHFFFAOYSA-N 0.000 claims description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 2
- JYVLIDXNZAXMDK-UHFFFAOYSA-N pentan-2-ol Chemical compound CCCC(C)O JYVLIDXNZAXMDK-UHFFFAOYSA-N 0.000 claims description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 2
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims 2
- 230000002378 acidificating effect Effects 0.000 claims 1
- 229940106691 bisphenol a Drugs 0.000 claims 1
- 235000013847 iso-butane Nutrition 0.000 claims 1
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 claims 1
- 150000002632 lipids Chemical class 0.000 claims 1
- 150000003151 propanoic acid esters Chemical class 0.000 claims 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N sec-butylidene Natural products CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 11
- 239000011248 coating agent Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 7
- 230000032050 esterification Effects 0.000 abstract description 5
- 238000005886 esterification reaction Methods 0.000 abstract description 5
- 239000006210 lotion Substances 0.000 description 16
- 239000003973 paint Substances 0.000 description 13
- 150000003254 radicals Chemical class 0.000 description 9
- 239000003921 oil Substances 0.000 description 8
- 235000019198 oils Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000002845 discoloration Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000012874 anionic emulsifier Substances 0.000 description 5
- ZQPPMHVWECSIRJ-MDZDMXLPSA-N elaidic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(O)=O ZQPPMHVWECSIRJ-MDZDMXLPSA-N 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229920000180 alkyd Polymers 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
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- 238000010438 heat treatment Methods 0.000 description 3
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- 238000005201 scrubbing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- UWHZIFQPPBDJPM-BQYQJAHWSA-N trans-vaccenic acid Chemical compound CCCCCC\C=C\CCCCCCCCCC(O)=O UWHZIFQPPBDJPM-BQYQJAHWSA-N 0.000 description 1
- 239000002383 tung oil Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 239000008170 walnut oil Substances 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/46—Polyesters chemically modified by esterification
- C08G63/48—Polyesters chemically modified by esterification by unsaturated higher fatty oils or their acids; by resin acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/08—Polyesters modified with higher fatty oils or their acids, or with natural resins or resin acids
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Paints Or Removers (AREA)
Abstract
Interior wall sealing wax aqueous alkide resin emulsion and preparation method thereof is provided, the method includes so that the binary acid of the unsaturated fatty acid of 30-60 weight %, the polyalcohol of 5-10 weight %, the trimethylolpropane of 10-15 weight %, 15-20 weight % is carried out esterification to acid value Jiang Zhi≤10mgKOH/g；At 175-180 DEG C, trimellitic anhydride is added to acid value 60-75mgKOH/g；At 80-90 DEG C, dimethylethanolamine, emulsifier and water mixing is added；The wherein described emulsifier is anion emulsifier and/or nonionic emulsifier, and the degree of branching of the emulsifier is 50%-90% or less.The interior wall sealing wax aqueous alkide resin emulsion excellent in stability of the present invention, while the excellent water resistance of the film of coating prepared therefrom.
Description
Technical field
The present invention relates generally to paint fields, more particularly to the interior wall sealing wax aqueous alkide resin that water resistance is excellent
Lotion and preparation method thereof.
Background technology
Current alkyd resin be still based on solvent type, still, with the development of economy with environmental protection requirement, by alkyd
Resin Water-borne modification has become development trend.
Aqueous alkide resin is mainly used in industrial sealing wax at present, and industrial sealing wax focuses on the performances such as anti-corrosion, the antirust of sealing wax.
Different from industrial sealing wax, interior wall sealing wax more focuses on the performances such as environmentally friendly, water-fast, scrubbing resistance.Therefore, to the aqueous alcoholic as adhesive
Acid resin requires higher.It is not specifically applied to the enhanced water resistance alkide resin emulsion of interior wall sealing wax still at present.
Invention content
In order to solve the above-mentioned technical problem, the present inventor has found after extensive studies it, by using specific outer
Add emulsifier, while realizing resin Water-borne modification, so as to get sealing wax after film forming have excellent water resistance.Specifically,
The present invention includes the following contents.
An aspect of of the present present invention provides the preparation method of interior wall sealing wax aqueous alkide resin emulsion comprising：
Make the trihydroxy methyl of the unsaturated fatty acid of 30-60 weight %, the polyalcohol of 5-10 weight %, 10-15 weight %
Propane, 15-20 weight % binary acid carry out esterification to acid value Jiang Zhi≤10mgKOH/g；
At 175-180 DEG C, trimellitic anhydride is added to acid value 60-75mgKOH/g；
At 80-90 DEG C, dimethylethanolamine is added, emulsifier is added under stiring later；
Water, stirring discharging are slowly added at 80-90 DEG C；
The wherein described emulsifier is anion emulsifier and/or nonionic emulsifier, and the degree of branching of emulsifier is 50%-
90%, wherein the degree of branching is calculate by the following formula：
Wherein " BP " is the degree of branching, and unit is percentage, and " a " is that have more than 2 reactive groups in each molecule
The total yield of polyfunctional monomer, " b " are the total yields of all monomers.
In certain embodiments, the anion emulsifier is formed by the monomer comprising carboxylic acid anhydride group or acid groups.
Preferably, the anion emulsifier include dihydromethyl propionic acid dioleate/salt and dihydromethyl propionic acid dilinoleic acid ester/
Salt.
In certain embodiments, the nonionic emulsifier is formed by the monomer comprising polyalkylene oxide groups.
Another aspect of the present invention provides interior wall sealing wax aqueous alkide resin emulsion, it includes it is as described above it is non-from
Sub- emulsifier and anion emulsifier.
Specific implementation mode
The existing various exemplary embodiment that the present invention will be described in detail, the detailed description are not considered as the limit to the present invention
System, and it is understood as the more detailed description to certain aspects of the invention, characteristic and embodiment.
It should be understood that heretofore described term is only to describe special embodiment, being not intended to limit this hair
It is bright.In addition, for the numberical range in the present invention, it is thus understood that it is also specifically disclosed that every between the upper and lower bound of the range
A median.Median and any other statement value in any statement value or stated ranges or in the range in
Between each of between value smaller range be also included in the present invention.These small range of upper and lower bounds can include independently
Or it excludes in range.
Unless otherwise stated, all technical and scientific terms used herein has the routine in field of the present invention
The normally understood identical meanings of technical staff.Although the present invention only describes preferred method and material, the present invention's
Implement or can also be used and similar or equivalent any method and material described herein in testing.The institute mentioned in this specification
There is document to be incorporated by reference into, to disclosure and description and the relevant method of the document and/or material.It is incorporated to any
When document conflicts, it is subject to the content of this specification.
In the present invention, vocabulary of terms had both included singulative, also included plural form, unless context separately clearly refers to
Go out.Heretofore described "at least one" refers not only to the case where comprising "one" or "an", and prior also includes " more
It is a " or the case where " a variety of ".
As used in the present invention, term " interior wall sealing wax " is sometimes referred to as " water paint for internal walls ", " interior wall water-based composition ",
Refer to the paint vehicle or coating painted on wall indoors.Compared with painting in outdoor exterior wall paint, paint film is softer, water-resistant capacity
It is weaker.
As used in the present invention, term " sealing wax " refers to the coating composition for being dispersed or dissolved in aqueous solvent.Including, but not
It is limited to water-reducible coating and Water-dispersing coatings (or water-dispersible paint).Lotion is emulsified after referring to as water-reducible coating is
The coating that film forming matter is prepared, can be diluted in construction with water.Emulsion is that instigate solvent type resin to be dissolved in organic molten after wherein
In agent, then make the lotion that resin dispersion is formed in water by strong mechanical agitation with the help of emulsifier.As moisture
Scattered coating refers to the coating prepared as film forming matter using synthetic resin emulsion.Lotion refers in the presence of emulsifier, in mechanical agitation
During, the small particles group that unsaturated ethylene alkenyl monomer is polymerized under the conditions of certain temperature is dispersed in water point of composition
Dissipate lotion.
As used in the present invention, term " degree of branching " is calculate by the following formula：
Wherein " BP " is the degree of branching, and unit is percentage, and " a " is that have more than 2 reactive groups in each molecule
The total yield of polyfunctional monomer, " b " are the total yields of all monomers.C.J.Hawker, R.Lee, J.M.J.Frechet,
J.Am.Chem.Soc.113 describes the analysis method that the degree of branching is described using NMR in 4583,1991, which is based on
Dendroid unit, end unit and linear unit measure numerical value.
If all monomers of emulsifier are all simple function and difunctionality, the degree of branching is necessarily 0%.On the other hand,
If the degree of functionality of all monomers of emulsifier is all 3 or more, the degree of branching is necessarily 100%.As polyfunctional monomer amount increases
Add, the degree of branching also increases.
Without being bound by theory, it has been recognised by the inventors that emulsifier when emulsion polymerization of the present invention is amphiphilic, i.e. there is parent in one end
Oiliness, the other end have hydrophily.Lower in the degree of branching, hydrophobic group can be more closely deposited in micella, together
When hydrophilic radical can more closely be deposited in outside micella.These emulsifiers still remain in lotion after the completion of polymerization, film forming
After remain in paint film, compared with the high emulsifier of the degree of branching, after meeting water hydrophilic group be easier with water act on, promote water painting
It more permeates, spread and migrates in film, increase water absorption rate.Thus the water resistance of the paint film to obtaining has an adverse effect.
Based on this, the inventors discovered that, it is 50% or more, preferably 60% or more in the degree of branching of emulsifier, more preferably
70% or more；On the other hand, be 90% hereinafter, when in more preferable 85% or less range, emulsifier be it is Slight branching, thus
The paint film of generation has higher water resistance.If the degree of branching is excessively high, the stability of emulsion generated is deteriorated.
As used in the present invention, term " nonionic emulsifier " refers to the breast formed by the monomer comprising polyalkylene oxide groups
Agent.The wherein described monomer comprising polyalkylene oxide groups does not include hydrophilic radical further preferably, or comprising a small amount of hydrophilic
Property group, for example, each monomer can have 0-4, preferably 0-2 hydrophilic radical.Because such as when the hydrophilic radical is
When acid groups, the dispersion of emulsifier in water, which is ionized by acid groups by reacting with alkali, to be influenced.As the parent
When aqueous group is acid anhydride, the dispersion of emulsifier in water is by anhydride group by polymerizeing to form adjacent two with polyol reaction
The influence of the open loop of anhydride group during the half ester of carboxylic acid.The free carboxy acid formed in the reaction is by with reacting for alkali
Ionization.
As used in the present invention, term " anion emulsifier " refers to being formed by the monomer comprising carboxylic acid anhydride group or acid groups
Emulsifier.The quantity of hydrophilic radical is 5-10, preferably 5-8 in wherein each monomer, for example, 6 or 7 reactive hydroxyl bases
Group.In certain embodiments, including the monomer of hydrophilic radical is glycol.
In certain embodiments, emulsifier is anionic emulsifier, includes hydrophilic radical by least one
Monomer and at least one ethylenic bond unsaturated fatty acid or ester copolyreaction and formed, wherein it is described at least one monomer
Including dihydromethyl propionic acid, dimethylolpropionic acid or combinations thereof.The example of such anionic emulsifier has dihydroxy first
Base propionic acid dioleate/salt and dihydromethyl propionic acid dilinoleic acid ester/salt.
In certain embodiments, emulsifier is by least one monomer comprising hydrophilic radical, the alkene
The copolyreaction of keyed unsaturated fatty acid or ester and at least one polyalcohol and formed；Wherein described at least one packet
Monomer containing hydrophilic radical includes primary alcohol alkoxylate, polyacid, carboxylic acid anhydrides or combinations thereof.In order to be introduced in emulsifier
A degree of branched, at least one polyalcohol may include at least three hydroxyl group.
In certain embodiments, emulsifier is the mixture of anionic emulsifier and nonionic emulsifier.It is preferred that
Ground, emulsifier of the invention are alkyd resin class emulsifiers.
As used in the present invention, term " unsaturated fatty acid " can be obtained in the form of natural oil, and the example includes, but unlimited
In Linseed oil (linseed oil), tung oil, poppy seed oil, perilla oil, walnut oil, coconut oil, palm oil, cotton seed oil, malt
Oil, soya-bean oil, olive oil, corn oil, sunflower oil, safflower oil, cannabis oil, canola oil, peanut oil, pilchard oil, and combinations thereof.No
Saturated fatty acid can also derive from dietary fat such as lard, duck oil and butter.Unsaturated fatty acid further includes myristoleic acid, palm fibre
Palmitic acid oleic acid, gaidic acid (sapienic acid), oleic acid, elaidic acid, vaccenic acid, erucic acid, linoleic acid, leukotrienes, anti-sub- oil
Sour (linoelaidic acid), alpha-linolenic acid, Pinolenic acid (pinolenic acid), arachidonic acid, eicosapentaenoic
Acid, erucic acid, docosahexaenoic acid, or combinations thereof.In certain embodiments, unsaturated fatty acid is oleic acid or leukotrienes.
In certain embodiments, it is 30-60%, example that the content of the unsaturated fatty acid, which is based on weight, when preparing lotion
Such as, 35%, 40%, 45%, 50%, 55% etc..
As used in the present invention, term " polyol " includes at least two hydroxyls.The polyalcohol can be for example, glycol,
Triol, tetrol or combinations thereof.In certain embodiments, the polyalcohol includes glycol and triol.Second of polyalcohol
Can be aliphatic, alicyclic or aromatics.The polyalcohol can be according to it to the pre- of the glass transition temperature (Tg) of emulsifier
Phase influences and selects.The example of the polyalcohol for being glycol have ethylene glycol, diethylene glycol (DEG), triethylene glycol, propylene glycol, dipropylene glycol,
1,2- butanediols, 2,3- butanediols, 1,3- propylene glycol, 1,4- butanediols, 1,5- pentanediols, neopentyl glycol, 1,6-HD, 3-
Methyl-1,5- pentanediols, 2- methyl -2,4-PD, 1,7- heptandiols, 2,2,4- trimethyl -1,3- pentanediols, 1,8- pungent two
Alcohol, 2,2- dimethyl -1,3- hexylene glycols, 1,4 cyclohexane dimethanol, catechol, resorcinol, hydroquinone and bisphenol-A.Institute
The example for stating the polyalcohol for being triol has glycerine, trimethylolethane, trimethylolpropane and tri hydroxy methyl butane.With higher
The example of the polyalcohol of degree of functionality has, pentaerythrite, dipentaerythritol and sorbierite.In certain embodiments, described polynary
Alcohol includes trimethylolpropane, 1,4 cyclohexane dimethanol, neopentyl glycol or combinations thereof.
In certain embodiments, prepare lotion when polyalcohol content be based on weight be 5-10%, for example, 6%, 7%,
8%, 9% etc..
As used in the present invention, term " water resistance " refers to the resistivity of effect of the paint film to water.It, which is measured, can be used this
Usually used any method in field, including, for example, room temperature submerging test method, leaching boiling test method, paint and varnish is water-fast
The measurement bowssening of property.As an example, the present invention provides following assay methods, i.e. GB/T 1733-93 paint films water resistance measuring method
(room temperature submerging test method).
Sample is immersed in normal-temperature water or boiling water, by observing coating surface variation after the testing time as defined in reaching
Phenomenon evaluates the water resistance of paint film.
Unless otherwise specified, test plate (panel) applies 1 before throwing examination:1 paraffin and rosin blend edge sealing, edge sealing width are 2-3mm.
Distilled water or deionized water are added in glass flume, unless otherwise specified, it is (23 ± 2) DEG C to adjust water temperature, and
The temperature is kept in the entire experiment process；Three pieces of test plate (panel)s are put into wherein, and make the 2/3 of every piece of test plate (panel) length to be soaked in water
In.
At the end of reaching soaking time as defined in product standard, test plate (panel) is taken out from slot, is blotted with filter paper, immediately or
To visually inspect test plate (panel) after being adjusted by time state as defined in product, and record whether loss of gloss, discoloration, blistering, wrinkle, get rusty
Phenomenon and recovery time.
In the present invention, organic solvent is not needed to prepare stable alkide resin emulsion.It can be optionally from stable alkyd tree
Organic solvent is excluded in fat liquor.Therefore, have in certain embodiments, using the total weight of interior wall aqueous alkide resin emulsion as base
Quasi- meter, the alkide resin emulsion include equal to or less than 2 weight %, particularly equal to or less than 1 weight %, be more specifically equal to
Or the organic solvent less than 0.5 weight %.In certain embodiments, organic solvent is not included.
Embodiment
The preparation of emulsifier
The preparation of the nonionic emulsifier of 1 present invention of embodiment
By sunflower oil (1750 grams), 350 grams of YMERTM N-120 (0.350 mole), 725 grams of PE (0.140 mole), 3.75
Gram MBTO and 3.75 gram of DBTO is placed in 5 liters of 3 neck round-bottom flasks, and the flask is cold equipped with the filling for the heating for being set as 95 DEG C
Condenser, mechanical agitator, thermocouple and nitrogen inlet.Reaction mixture is heated 8 hours at 210 DEG C, is then cooled to room temperature.
Phthalic anhydride (600 grams, 4.05 moles), 400 grams of M-phthalic acids (2.41 moles) and 50 milliliters of dimethylbenzene are added.It will be cold
Condenser is substituted for the Dean-Stark cold-trap that top carries Friedrichs condensers, and reaction mixture is heated at 220 DEG C.Make anti-
It should proceed to until acid value reaches about 11.0.The degree of branching of the emulsifier is 84%.
Comparative example 1 compares the preparation with anionic emulsifier
Under a nitrogen by 20.0 grams of UNOXOLTM glycol (0.14 mole), 19.0 grams of TMP (0.14 mole), 80.0 grams of NPG
(1.54 moles), 152.0 grams of phthalic anhydrides (1.03 moles) and 90.0 grams of linoleic acid (PAMOLYNTM200,1.43 moles)
Mixture stirred 8 hours at 200 DEG C.Temperature is reduced to 150 DEG C, and continues stirring until acid value is close to 28 milligrams of KOH/
Gram.Final acid value is 25-30 milligrams KOH/ grams, and Mn is about that 1900, PDI is about 2-3.This anionic of suitable alkali neutralization can be used
Emulsifier.Its degree of branching is 9%.
The preparation of comparative example 2-3 and embodiment 2-4 nonionics+anionic emulsifier
Emulsifier prepared by embodiment 1 is mixed in proportion with emulsifier prepared by comparative example 1, preparing the degree of branching respectively is
20% emulsifier (comparative example 2), 30% emulsifier (comparative example 3), 56% emulsifier (embodiment 2), 60% emulsification
Agent (embodiment 3), 75% emulsifier (embodiment 4).
The preparation of lotion
The preparation of 5 lotion 1 of the present invention of embodiment
Formula：
Oleic acid 40%, neopentyl glycol 8%, trimethylolpropane 11%, adipic acid 15%, trimellitic anhydride 5%, emulsifier
8%, water 50%, dimethylethanolamine 2%.
It is as follows：
(1) oleic acid, neopentyl glycol, trimethylolpropane, adipic acid are added in reaction kettle, cover pot cover；
(2) start to stir after temperature of reaction kettle being risen to 130-140 DEG C in 1-1.5h, while being passed through CO2 and condensed water；
(3) temperature of reaction kettle is risen into 178-182 DEG C, and esterification 0.8- at this temperature in 0.8-1.2h
1.2h；
(4) after the completion of esterification, temperature of reaction kettle is risen to 215-220 DEG C in 0.8-1.2h, keeps esterification later
Until reactant is fully transparent；
(5) after reactant is fully transparent in step (4), the measurement of an acid value is periodically carried out to reactant, works as acid value
Jiang Zhi≤10mgKOH/g stop heating and logical cooling water cool down；
(6) when temperature is down to 175-180 DEG C, trimellitic anhydride is added and is kept to acid value 60- in 175-180 DEG C
75mgKOH/g stops heating and leads to cooling water temperature；
(7) it is cooled to after 80-90 DEG C, stops CO2Be passed through, be added dimethylethanolamine stir evenly；
(8) 80-90 DEG C of temperature is kept, the emulsifier of embodiment 1 is added, stirs evenly；
(9) material maintains 80-90 DEG C, is slowly added to 80-90 DEG C of warm water, and high-speed stirred discharges for 30 minutes.
The preparation of embodiment 6-8 lotions of the present invention
Other than the emulsifier 1 in embodiment 5 is replaced with the emulsifier in embodiment 2-4 respectively, with embodiment 5
Identical mode prepares the lotion 2-4 of the present invention.
Comparative example 4-6 compares the preparation with lotion
Other than the emulsifier 1 in embodiment 5 is replaced with the emulsifier in comparative example 2-3 respectively, with embodiment 5
Prepared by identical mode compares with lotion 2-3.
The preparation of coating
Corresponding coating is prepared by following formulas (parts by weight)：
300 parts of water, 90 parts of interior wall anatase thpe white powder, 3 parts of hydroxyethyl cellulose, 5 parts of dispersant, 5 parts of antifoaming agent, wetting
3 parts of agent, 300 parts of coarse whiting, 3 parts of sterilization antiseptic, 5 parts of thickener, 200 parts of aqueous alkide resin emulsion.
Wherein aqueous alkide resin emulsion is selected respectively as lotion 1-4 of the present invention and is compared with lotion 1-3.
Table 1
Note：
It is excellent：No loss of gloss, discoloration, blistering and corrugation occur；
It is good：No discoloration, blistering and corrugation occur, but slightly loss of gloss；
It is good：Occur without blistering, corrugation, but slightly loss of gloss and discoloration；
Difference：Loss of gloss, discoloration are serious；
It is poor：Loss of gloss, discoloration and blistering；
It is very poor：Loss of gloss, discoloration, blistering and corrugation.
Without departing substantially from the scope or spirit of the invention, the specific implementation mode of description of the invention can be done more
Kind is improved and variation, this will be apparent to those skilled in the art.Other realities obtained by the specification of the present invention
It is apparent obtain to apply mode for technical personnel.Present specification and embodiment are merely exemplary.
Claims (9)
1. a kind of preparation method of interior wall sealing wax aqueous alkide resin emulsion comprising：Make the unsaturated lipid of 30-60 weight %
Fat acid, the polyalcohol of 5-10 weight %, the trimethylolpropane of 10-15 weight %, 15-20 weight % adipic acid be esterified
It reacts to acid value Jiang Zhi≤10mgKOH/g；
At 175-180 DEG C, trimellitic anhydride is added to acid value 60-75mgKOH/g；
At 80-90 DEG C, dimethylethanolamine, emulsifier and water stirring is added；
The wherein described emulsifier is anion emulsifier and/or nonionic emulsifier, and the degree of branching of the emulsifier is 50%-
90%, wherein the degree of branching is calculate by the following formula：
Wherein " BP " is the degree of branching, and unit is percentage, and " a " is the more officials having in each molecule more than 2 reactive groups
The total yield of energy monomer, " b " is the total yield of all monomers；
Wherein, the polyalcohol is ethylene glycol, diethylene glycol (DEG), triethylene glycol, propylene glycol, dipropylene glycol, 1,2- butanediols, 2,3- fourths two
Alcohol, 1,3- propylene glycol, 1,4- butanediols, 1,5- pentanediols, neopentyl glycol, 1,6-HD, 3- methyl-1s, 5- pentanediols, 2-
Methyl -2,4-PD, 1,7- heptandiols, 2,2,4- trimethyl -1,3- pentanediols, 1,8- ethohexadiols, 2,2- dimethyl -1,3-
Hexylene glycol, 1,4 cyclohexane dimethanol, catechol, resorcinol, hydroquinone, bisphenol-A, glycerine, trimethylolethane, three hydroxyls
Methylpropane, tri hydroxy methyl butane, pentaerythrite, dipentaerythritol, sorbierite, trimethylolpropane, 1,4- hexamethylene diformazans
Alcohol or neopentyl glycol.
2. preparation method according to claim 1, wherein the degree of branching of the emulsifier is 55%-85%.
3. preparation method according to claim 1, wherein the degree of branching of the emulsifier is 60%.
4. preparation method according to claim 1, wherein the anion emulsifier is by including carboxylic acid anhydride group or acidic group
The monomer of group is formed.
5. preparation method according to claim 1, wherein the anion emulsifier includes two oleic acid of dihydromethyl propionic acid
Ester/salt or dihydromethyl propionic acid dilinoleic acid ester/salt.
6. preparation method according to claim 1, wherein the nonionic emulsifier is by the list comprising polyalkylene oxide groups
Body is formed.
7. according to claim 1-6 any one of them preparation methods, wherein the unsaturated fatty acid is oleic acid.
8. according to claim 1-6 any one of them preparation methods, wherein the polyalcohol is neopentyl glycol.
9. a kind of interior wall sealing wax aqueous alkide resin emulsion, it includes emulsifier, the emulsifier be anion emulsifier and/
Or nonionic emulsifier, and the degree of branching of the emulsifier is 50%-90%, wherein the degree of branching is calculate by the following formula：
Wherein " BP " is the degree of branching, and unit is percentage, and " a " is the more officials having in each molecule more than 2 reactive groups
The total yield of energy monomer, " b " is the total yield of all monomers.
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| CN101348604A (en) * | 2008-09-05 | 2009-01-21 | 中国海洋石油总公司 | Aqueous alkide resin emulsion and preparation thereof |
| CN102604517A (en) * | 2012-02-29 | 2012-07-25 | 长兴化学工业(中国)有限公司 | High-performance aqueous alkyd resin paint |
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| CN102127213B (en) * | 2011-01-17 | 2013-05-22 | 华中科技大学 | Waterborne acrylic alkyd resin and preparation method and application thereof |
| CN104530398A (en) * | 2014-12-04 | 2015-04-22 | 北京金汇利应用化工制品有限公司 | Waterborne alkyd resin and aqueous dispersion thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101348604A (en) * | 2008-09-05 | 2009-01-21 | 中国海洋石油总公司 | Aqueous alkide resin emulsion and preparation thereof |
| CN102604517A (en) * | 2012-02-29 | 2012-07-25 | 长兴化学工业(中国)有限公司 | High-performance aqueous alkyd resin paint |
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