CN106866950A - 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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- CN106866950A CN106866950A CN201710017411.5A CN201710017411A CN106866950A CN 106866950 A CN106866950 A CN 106866950A CN 201710017411 A CN201710017411 A CN 201710017411A CN 106866950 A CN106866950 A CN 106866950A
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- acid
- emulsifying agent
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- 239000000839 emulsion Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 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
- 238000004945 emulsification Methods 0.000 title abstract description 5
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 60
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002253 acid Substances 0.000 claims abstract description 32
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- 150000001450 anions Chemical group 0.000 claims abstract description 10
- 239000012875 nonionic emulsifier Substances 0.000 claims abstract description 9
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000032050 esterification Effects 0.000 claims abstract description 6
- 238000005886 esterification reaction Methods 0.000 claims abstract description 6
- 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
- 239000000178 monomer Substances 0.000 claims description 25
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
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- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 6
- -1 propionic acid dilinoleic acid ester Chemical class 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
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- 239000003973 paint Substances 0.000 description 14
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- 238000005187 foaming Methods 0.000 description 5
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- 239000000463 material Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 3
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- 238000010998 test method Methods 0.000 description 3
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
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- HXQHFNIKBKZGRP-UHFFFAOYSA-N Ranuncelin-saeure-methylester Natural products CCCCCC=CCC=CCCC=CCCCC(O)=O HXQHFNIKBKZGRP-UHFFFAOYSA-N 0.000 description 2
- 235000019486 Sunflower oil Nutrition 0.000 description 2
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- 150000008064 anhydrides Chemical group 0.000 description 2
- YZXBAPSDXZZRGB-DOFZRALJSA-N arachidonic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O YZXBAPSDXZZRGB-DOFZRALJSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
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- 239000000498 cooling water Substances 0.000 description 2
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- DPUOLQHDNGRHBS-KTKRTIGZSA-N erucic acid Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(O)=O DPUOLQHDNGRHBS-KTKRTIGZSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 2
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- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 description 1
- 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 description 1
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- 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 description 1
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- 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
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-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
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)
- Paints Or Removers (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
Interior wall sealing wax aqueous alkide resin emulsion and preparation method thereof is provided, methods described includes making the unrighted acid of 30 60 weight %, the polyalcohol of 5 10 weight %, the trimethylolpropane of 10 15 weight %, the binary acid of 15 20 weight % carry out esterification to acid value Jiang Zhi≤10mgKOH/g;At 175 180 DEG C, trimellitic anhydride to the 75mgKOH/g of acid value 60 is added;At 80 90 DEG C, the mixing of dimethylethanolamine, emulsifying agent and water is added;Wherein described emulsifying agent is anion emulsifier and/or nonionic emulsifier, and the degree of branching of the emulsifying agent is for below 50% 90%.Interior wall sealing wax aqueous alkide resin emulsion excellent in stability of the invention, while the excellent water resistance of the film of coating prepared therefrom.
Description
Technical field
The present invention relates generally to paint field, more particularly to the interior wall sealing wax aqueous alkide resin that water resistance is excellent
Emulsion and preparation method thereof.
Background technology
Current alkyd resin be still based on solvent-borne type, but, with expanding economy and environmental protection requirement, by alkyd
Resin Water-borne modification has turned into 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 performance such as environmentally friendly, water-fast, scrubbing resistance.Therefore, to the aqueous alcoholic as adhesive
Acid resin requirement is higher.It is not specifically applied to the enhanced water resistance alkide resin emulsion of interior wall sealing wax still at present.
The content of the invention
In order to solve the above-mentioned technical problem, the present inventor has found after extensive studies it, by using specific outer
Plus emulsifying agent, while resin Water-borne modification is realized, so as to get sealing wax after film forming have excellent water resistance.Specifically,
The present invention includes herein below.
An aspect of of the present present invention, there is provided the preparation method of interior wall sealing wax aqueous alkide resin emulsion, it includes:
Make unrighted acid, the polyalcohol of 5-10 weight %, the trihydroxy methyl of 10-15 weight % of 30-60 weight %
Propane, the binary acid of 15-20 weight % carry out esterification to acid value Jiang Zhi≤10mgKOH/g;
At 175-180 DEG C, trimellitic anhydride to acid value 60-75mgKOH/g is added;
At 80-90 DEG C, dimethylethanolamine is added, add emulsifying agent under agitation afterwards;
Water, stirring discharging are slowly added at 80-90 DEG C;
Wherein described emulsifying agent is anion emulsifier and/or nonionic emulsifier, and the degree of branching of emulsifying agent is 50%-
90%, wherein the degree of branching is calculated by 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 " is the total yield 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 comprising 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, there is provided interior wall sealing wax aqueous alkide resin emulsion, its include it is as described above it is non-from
Sub- emulsifying agent and anion emulsifier.
Specific embodiment
Now describe various exemplary implementation method of the invention in detail, the detailed description is not considered as to limit of the 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 implementation method, being not intended to limit this hair
It is bright.In addition, for the number 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 scope
Individual median.Median and any other statement value in any statement value or stated ranges or in the scope in
Between each less scope between value be also included in the present invention.These small range of upper and lower bounds can independently include
Or exclude in the range of.
Unless otherwise stated, all technologies used herein and scientific terminology have the routine in field of the present invention
The identical meanings that technical staff is generally understood that.Although the present invention only describes preferred method and material, of the invention
Implement or can also be used and similar or equivalent any method described herein and material in testing.The institute mentioned in this specification
There is document to be incorporated by reference into, to the disclosure and description method related to the document and/or material.It is incorporated to any
When document conflicts, it is defined by the content of this specification.
In the present invention, vocabulary of terms both includes singulative, also including plural form, unless context separately clearly refers to
Go out.Heretofore described " at least one " refers not only to the situation comprising " one " or " one kind ", prior also comprising " many
It is individual " or " various " situation.
As used in the present invention, term " interior wall sealing wax " is sometimes referred to as " water paint for internal walls ", " interior wall waterborne compositions ",
Refer to the paint vehicle or coating painted on wall indoors.Compared with painting in outdoor exterior wall paint, its 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).Emulsion 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 to instigate solvent type resin to be dissolved in organic molten after wherein
In agent, the emulsion for then leaning on strong mechanical agitation to make resin dispersion be formed in water with the help of emulsifying agent.As moisture
Scattered coating refers to the coating prepared as film forming matter with synthetic resin emulsion.Emulsion refers in the presence of emulsifying agent, in mechanical agitation
During, the small particles group that unsaturated ethylene alkenyl monomer is polymerized under the conditions of uniform temperature is dispersed in water dividing for composition
Dissipate emulsion.
As used in the present invention, term " degree of branching " is calculated by 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 " is the total yield of all monomers.C.J.Hawker, R.Lee, J.M.J.Frechet,
J.Am.Chem.Soc.113, describes to describe the analysis method of the degree of branching using NMR in 4583,1991, and the degree of branching is based on
Dendroid unit, end unit and linear unit measure numerical value.
If all monomers of emulsifying agent 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 emulsifying agent is all more than 3, the degree of branching is necessarily 100%.As polyfunctional monomer amount increases
Plus, the degree of branching also increases.
Without being bound by theory, it has been recognised by the inventors that emulsifying agent during emulsion polymerization of the present invention is amphiphilic, i.e. there is parent one end
Oiliness, the other end has hydrophily.In the case where the degree of branching is relatively low, hydrophobic group more closely can be deposited in micella, together
When hydrophilic radical more closely can be deposited in outside micella.During these emulsifying agents still remain in emulsion after the completion of polymerization, film forming
After remain in paint film, compared with degree of branching emulsifying agent high, meet water after hydrophilic group be easier with water act on, promote water paint
More permeated in film, spread and migrated, increase water absorption rate.Thus the water resistance of the paint film to obtaining has a negative impact.
Based on this, the inventors discovered that, it is more than 50%, preferably more than 60% in the degree of branching of emulsifying agent, more preferably
More than 70%;On the other hand, be less than 90%, when in more preferably less than 85% scope, emulsifying agent be it is Slight branching, thus
The paint film of generation has water resistance higher.If the degree of branching is too high, the stability of emulsion for producing 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 for example when the hydrophilic radical is
During acid groups, dispersion of the emulsifying agent in water is by acid groups by being reacted with alkali and ionizing is influenceed.As the parent
When aqueous group is acid anhydride, dispersion of the emulsifying agent in water to be formed adjacent two so as to be polymerized by anhydride group by with polyol reaction
The influence of the open loop of anhydride group during the half ester of carboxylic acid.The free carboxy acid for being formed in the reaction is by the reaction with alkali
Ionization.
As used in the present invention, term " anion emulsifier " refers to be formed by the monomer comprising carboxylic acid anhydride group or acid groups
Emulsifying agent.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, the monomer comprising hydrophilic radical is glycol.
In certain embodiments, emulsifying agent is anionic emulsifier, and it passes through at least one comprising hydrophilic radical
Monomer and at least one ethylenic unrighted acid or ester copolyreaction and formed, wherein at least one monomer
Including dihydromethyl propionic acid, dimethylolpropionic acid or its combination.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, emulsifying agent is by least one monomer comprising hydrophilic radical, the alkene
The copolyreaction of keyed unrighted acid or ester and at least one polyalcohol and formed;Wherein described at least one bag
Monomer containing hydrophilic radical includes primary alcohol alkoxylate, polyacid, carboxylic acid anhydrides or its combination.In order to be introduced in emulsifying agent
A certain degree of branched, at least one polyalcohol can include at least 3 oh groups.
In certain embodiments, emulsifying agent is the mixture of anionic emulsifier and nonionic emulsifier.It is preferred that
Ground, emulsifying agent of the invention is alkyd resin class emulsifying agent.
As used in the present invention, term " unrighted acid " can be obtained in the form of natural oil, and the example includes, but does not limit
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.Unrighted acid also 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, DHA or its combination.In certain embodiments, unrighted acid is oleic acid or leukotrienes.
In certain embodiments, it is 30-60%, example that the content of the unrighted acid is based on weight when preparing emulsion
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 its combination.In certain embodiments, the polyalcohol includes glycol and triol.Second polyalcohol
Can be aliphatic, alicyclic or aromatics.The polyalcohol can be according to it to emulsifying agent glass transition temperature (Tg) it is pre-
Phase influences and selects.The example of the polyalcohol for being glycol have ethylene glycol, diethylene glycol (DEG), triethylene glycol, propane diols, dipropylene glycol,
1,2- butanediols, 2,3- butanediols, 1,3- propane diols, 1,4- butanediols, 1,5- pentanediols, neopentyl glycol, 1,6-HD, 3-
Methyl isophthalic acid, 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, hydroquinones and bisphenol-A.Institute
Stating the example of 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, it is described polynary
Alcohol includes trimethylolpropane, 1,4 cyclohexane dimethanol, neopentyl glycol or its combination.
In certain embodiments, prepare emulsion when polyalcohol content be based on weight be 5-10%, for example, 6%, 7%,
8%th, 9% etc..
As used in the present invention, term " water resistance " refers to resistivity of the paint film to the effect of water.Its measure can be using this
Usually used any method in field, including, for example, normal temperature submerging test method, leaching boiling test method, paint and varnish is water-fast
The measure bowssening of property.As an example, the present invention provides following assay methods, i.e. GB/T 1733-93 paint films water resistance determination method
(normal temperature submerging test method).
Sample is immersed in normal-temperature water or boiling water, is changed by observing coating surface after the testing time for reaching regulation
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 is 2-3mm.
Distilled water or deionized water are added in glass flume, unless otherwise specified, regulation water temperature is (23 ± 2) DEG C, and
The temperature is kept in whole experiment process;Three pieces of test plate (panel)s are put into wherein, and make every piece the 2/3 of test plate (panel) length to be soaked in water
In.
At the end of the soak time that product standard specifies is reached, test plate (panel) is taken out from groove, is blotted with filter paper, immediately or
The time state specified by product adjust after to visually inspect test plate (panel), and record whether loss of gloss, change colour, bubble, wrinkling, getting rusty
Phenomenon and recovery time.
In the present invention, it is not necessary to organic solvent come prepare stabilization alkide resin emulsion.Can optionally from the alkyd tree of stabilization
Organic solvent is excluded in fat liquor.Therefore, have in some embodiments, the gross weight with interior wall aqueous alkide resin emulsion is as base
Quasi- meter, the alkide resin emulsion includes and is equal to or less than 2 weight %, especially equal or less than 1 weight %, is more specifically equal to
Or less than the organic solvent of 0.5 weight %.In certain embodiments, not comprising organic solvent.
Embodiment
The preparation of emulsifying agent
The preparation of the nonionic emulsifier of the invention of embodiment 1
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 of the heating for being set as 95 DEG C
Condenser, mechanical agitator, thermocouple and nitrogen inlet.Reactant mixture is heated 8 hours at 210 DEG C, room temperature is then cooled to.
Add phthalic anhydride (600 grams, 4.05 moles), 400 grams of M-phthalic acids (2.41 moles) and 50 milliliters of dimethylbenzene.Will be cold
Condenser is substituted for Dean-Stark cold-trap of the top with Friedrichs condensers, in 220 DEG C of heating response mixtures.Make anti-
Should proceed to untill acid number reaches about 11.0.The degree of branching of the emulsifying agent is 84%.
Comparative example 1 compares with the preparation of 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 number close to 28 milligrams of KOH/
Gram.Final acid number is 25-30 milligrams KOH/ grams, and Mn is about 1900, PDI and is about 2-3.This anionic can be neutralized with suitable alkali
Emulsifying agent.Its degree of branching is 9%.
The preparation of comparative example 2-3 and embodiment 2-4 nonionics+anionic emulsifier
The emulsifying agent that emulsifying agent prepared by embodiment 1 is prepared with comparative example 1 mixes in proportion, the degree of branching is prepared respectively and is
20% emulsifying agent (comparative example 2), 30% emulsifying agent (comparative example 3), 56% emulsifying agent (embodiment 2), 60% emulsification
Agent (embodiment 3), 75% emulsifying agent (embodiment 4).
The preparation of emulsion
The preparation of the emulsion 1 of the present invention of embodiment 5
Formula:
Oleic acid 40%, neopentyl glycol 8%, trimethylolpropane 11%, adipic acid 15%, trimellitic anhydride 5%, emulsifying agent
8%th, water 50%, dimethylethanolamine 2%.
Comprise the following steps that:
(1) oleic acid, neopentyl glycol, trimethylolpropane, adipic acid are added in reactor, covers pot cover;
(2) stirring is started after temperature of reaction kettle being risen into 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, esterification is kept afterwards
Until reactant is fully transparent;
(5) after reactant is fully transparent in step (4), a measure for acid value is regularly carried out to reactant, works as acid value
Jiang Zhi≤10mgKOH/g, stopping is heated and leads to cooling water and lowered the temperature;
(6) when temperature is down to 175-180 DEG C, trimellitic anhydride is added to be kept to acid value 60- in 175-180 DEG C
75mgKOH/g, stops the logical cooling water temperature of heating;
(7) it is cooled to 80-90 DEG C afterwards, stops CO2Be passed through, add dimethylethanolamine stir;
(8) 80-90 DEG C of keeping temperature, adds the emulsifying agent of embodiment 1, stirs;
(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 emulsions of the present invention
In addition to the emulsifying agent during the emulsifying agent 1 in embodiment 5 is replaced with into embodiment 2-4 respectively, with embodiment 5
Identical mode prepares emulsion 2-4 of the invention.
Comparative example 4-6 compares with the preparation of emulsion
In addition to the emulsifying agent during the emulsifying agent 1 in embodiment 5 is replaced with into comparative example 2-3 respectively, with embodiment 5
Identical mode prepares to compare uses emulsion 2-3.
The preparation of coating
Corresponding coating is prepared by following formulas (weight portion):
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 defoamer, 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 uses emulsion 1-3 with comparing from for emulsion 1-4 of the present invention respectively.
Table 1
Note:
It is excellent:Occur without loss of gloss, discoloration, foaming and corrugation;
It is good:Occur without discoloration, foaming and corrugation, but somewhat loss of gloss;
It is good:Occur without foaming, corrugation, but somewhat loss of gloss and discoloration;
Difference:Loss of gloss, discoloration are serious;
It is poor:Loss of gloss, discoloration and foaming;
It is very poor:Loss of gloss, discoloration, foaming and corrugation.
In the case of without departing substantially from the scope of the present invention or spirit, can do many to the specific embodiment of description of the invention
Plant and improve and change, this will be apparent to those skilled in the art.Other realities obtained by specification of the invention
It is for technical personnel apparent obtaining to apply mode.Present specification and embodiment are only exemplary.
Claims (10)
1. a kind of preparation method of interior wall sealing wax aqueous alkide resin emulsion, it includes:
Make the unrighted acid of 30-60 weight %, the polyalcohol of 5-10 weight %, the trimethylolpropane of 10-15 weight %,
The binary acid of 15-20 weight % carries out esterification to acid value Jiang Zhi≤10mgKOH/g;
At 175-180 DEG C, trimellitic anhydride to acid value 60-75mgKOH/g is added;
At 80-90 DEG C, the stirring of dimethylethanolamine, emulsifying agent and water is added;
Wherein described emulsifying agent is anion emulsifier and/or nonionic emulsifier, and the degree of branching of the emulsifying agent is 50%-
90%, wherein the degree of branching is calculated by following formula:
Wherein " BP " is the degree of branching, and unit is percentage, and " a " is that have more than 2 many officials of reactive group in each molecule
The total yield of energy monomer, " b " is the total yield of all monomers.
2. preparation method according to claim 1, wherein the degree of branching of the emulsifying agent is 55%-85%.
3. preparation method according to claim 1, wherein the degree of branching of the emulsifying agent is 60%.
4. preparation method according to claim 1, wherein the anion emulsifier is by comprising 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 the oleic acid of dihydromethyl propionic acid two
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. the preparation method according to claim any one of 1-6, wherein the unrighted acid is oleic acid.
8. the preparation method according to claim any one of 1-6, wherein the polyalcohol is neopentyl glycol.
9. the preparation method according to claim any one of 1-6, wherein the binary acid is adipic acid.
10. a kind of interior wall sealing wax aqueous alkide resin emulsion, it includes emulsifying agent, and the emulsifying agent is anion emulsifier
And/or nonionic emulsifier, and the degree of branching of the emulsifying agent is 50%-90%, wherein the degree of branching is calculated by following formula:
Wherein " BP " is the degree of branching, and unit is percentage, and " a " is that have more than 2 many officials of reactive group in each molecule
The total yield of energy monomer, " b " is the total yield of all monomers.
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CN104845510A (en) * | 2014-12-04 | 2015-08-19 | 北京金汇利应用化工制品有限公司 | Paint containing waterborne alkyd resin and preparation method of paint |
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CN115651173A (en) * | 2022-11-15 | 2023-01-31 | 亚士创能科技(乌鲁木齐)有限公司 | Bio-based waterborne alkyd resin and preparation method and application thereof |
CN115651173B (en) * | 2022-11-15 | 2024-02-06 | 亚士创能科技(乌鲁木齐)有限公司 | Bio-based water-based alkyd resin and preparation method and application thereof |
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