CN106589334B - Method of the fatty acid methyl Lipase absobed from dry water soluble alkyd resin - Google Patents
Method of the fatty acid methyl Lipase absobed from dry water soluble alkyd resin Download PDFInfo
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- CN106589334B CN106589334B CN201611186281.XA CN201611186281A CN106589334B CN 106589334 B CN106589334 B CN 106589334B CN 201611186281 A CN201611186281 A CN 201611186281A CN 106589334 B CN106589334 B CN 106589334B
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- 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
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- 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
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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Abstract
The invention discloses a kind of fatty acid methyl Lipase absobeds from the method for dry water soluble alkyd resin, using the fatty acid methyl ester of waste grease production as major ingredient, and design proportion dispensing is pressed with linoleic acid, pentaerythrite, ethylene glycol, terephthalic acid (TPA), benzoic acid, trimellitic anhydride, organotin, white lime, triethylamine, propandiol butyl ether；Reaction kettle first is added in fatty acid methyl ester, white lime is added after being preheating to about 140 DEG C and pentaerythrite is added when being warming up to about 190 DEG C, it is warming up to about 235 DEG C again and keeps the temperature 1.5 hours, linoleic acid, terephthalic acid (TPA), ethylene glycol, benzoic acid and organotin are added after no methanol steams, is kept the temperature then at about 230 DEG C；It is cooled to 180 DEG C of addition trimellitic anhydrides when being reacted to acid value less than 6, is cooled to 100 DEG C again after about 170 DEG C of heat preservations to acid value and viscosity qualification hereinafter, triethylamine and propandiol butyl ether is successively added, filtering gained filtrate is from dry water soluble alkyd resin.The present invention, which prepares water soluble alkyd resin, has the characteristics that low manufacture cost, dryness are good and with high hardness.
Description
Technical field
The present invention relates to the preparation methods from dry water soluble alkyd resin, and in particular to certainly dry using fatty acid methyl Lipase absobed
The method of water soluble alkyd resin.
Background technology
With the rapid development of economy, ecological environment is worsening, haze dust etc. causes air quality to be deteriorated, people couple
Environmental issue is increasingly paid close attention to.In order to reinforce environmental protection, various countries formulate environmental legislation to volatile organic compounds (VOC)
Discharge limits.About containing 50% organic solvent in solvent based coating traditional at present, in coating material production and work progress
In, a large amount of VOC is discharged into air, directly endangers the health of the mankind and other biological, thus industrially developed country opens
Begin a large amount of exploitation solid resins and water soluble alkyd resin, and existing water soluble alkyd resin and usual vehicle type alkyd
Coating comparison affects industrialized production and the marketization there are cost of manufacture height, dryness the difference deficiency low with hardness.
Invention content
The object of the present invention is to provide a kind of using fatty acid methyl Lipase absobed from the method for dry water soluble alkyd resin, solves
The defect that existing water soluble alkyd resin cost of manufacture is high, dryness difference is low with hardness.
In order to achieve the above object, fatty acid methyl Lipase absobed of the present invention utilizes abandoned oil from the method for dry water soluble alkyd resin
The fatty acid methyl ester of fat production is Material synthesis from dry water soluble alkyd resin, supplementary material fatty acid methyl ester 21 by mass percentage
~36%, linoleic acid 4~6%, pentaerythrite 7~9%, ethylene glycol 5~7%, terephthalic acid (TPA) 15~17%, benzoic acid 2~
4%, trimellitic anhydride 7~9%, organotin 0.7~1.4 ‰, white lime 0.12~0.2 ‰, triethylamine 3~5%, propylene glycol fourth
The proportioning of ether 20~22% prepares；Steps are as follows for synthetic operation：
(1) fatty acid methyl ester is added into reaction kettle, white lime is added after being preheating to 120~160 DEG C and continues to heat；
(2) pentaerythrite is added when being warming up to 180~200 DEG C, continues to heat up；
(3) when heat preservation 1~2 is small after temperature reaches 230~240 DEG C, linoleic acid is added after no methanol steams, to benzene two
Formic acid, ethylene glycol, benzoic acid and organotin are kept the temperature at a temperature of 220~240 DEG C；
(4) start to cool down when being reacted to acid value less than 6, trimellitic anhydride is added when temperature is down to 180 DEG C, in
Heat preservation to acid value is 36~42 at a temperature of 168~174 DEG C, viscosity is format (7：3) continue to cool down after 20~30s/25 DEG C；
(5) triethylamine and propandiol butyl ether are successively added after temperature is down to 100 DEG C or less, filtering is spare, and filtrate is
From dry water soluble alkyd resin.
The present invention has following technical characteristics：
1, Gao Jufa is used in technique, can effectively improve the dryness of aqueous alkide resin.
2, there are following characteristics in raw material selection：
Main film forming matter：Fatty acid methyl ester using waste grease production is that cost of material is low；
Polyalcohol：Using the pentaerythrite of rigid structure, ethylene glycol；Trimethylolpropane and neopentyl glycol, but it is of high cost,
It does not select；
Polyacid：Terephthalic acid (TPA) resistant to hydrolysis is good, at low cost, has better anti-ultraviolet property than phthalic anhydride；Isophthalic diformazan
Acid value lattice double than terephthalic acid (TPA), do not select；
Water-borne modification raw material：Trimellitic anhydride (TMA), dihydromethyl propionic acid (DMPA), 5-sodium sulfo isophthalate (5-
SSIPA), latter two is not only of high cost, but also synthetic resin complex process, from solid carbon dioxide dissolubility phthalic resin coating poor performance, only
It is suitble to production amino-stoving varnish water soluble alkyd resin, does not select herein；Trimellitic anhydride not only provides the water solubility of resin, also
Effectively improve hardness of paint film.
It is designed using linearity molecular structure on water soluble alkyd resin molecular structure, avoids using K values and alcohol excess R, make
Resin structure is regular, it is anti-it is dry return viscous hydroxyl value control in 18-30mg/g, secondly trimellitic anhydride is not pre- on the end group of resin
Two carboxyls are stayed, but on molecular structure, a carboxyl is only provided, filming performance final in this way could be best.
Water soluble alkyd resin molecular structure is：
R represents aliphatic acid；
+ represent pentaerythrite；
Represent ethylene glycol；
Represents terephthalic acid (TPA)；
Represent trimellitic anhydride；
Δ represents benzoic acid.
Its-COOH offers achieve the purpose that water-soluble with amine or ammonia neutralization.
Fatty acid methyl Lipase absobed of the present invention from the method for dry water soluble alkyd resin prepare from dry water soluble alkyd resin
It is shown in Table 1 with the comparison of solvent-borne alkyd resins technical indicator.
1 water soluble alkyd resin of table is compared with solvent-borne alkyd resins technical indicator
Table 1 can be seen that：
A, acid value is different, and it is water-soluble that water soluble alkyd resin, which reaches water-soluble key condition, this TMA system is determined with acid value
It is fixed water-soluble.Good water solubility but water-fast difference when excessively high；It is in emulsus or not soluble in water when too low, is not easy to scrub and clean.
B, solid content % determines the content of organic volatile solvent, it was demonstrated that water-soluble one times fewer than solvent type.
C, dryness：Surface drying (doing solid work) all it is faster than solvent type very much.
D, hardness：It is also more much higher than solvent type.
In conclusion the performance ratio solvent-borne alkyd resins of water soluble alkyd resin is good.
By taking iron oxide red water-soluble alcohol acid antirust paint as an example, prepared from dry water soluble alkyd resin from dry using prepared by the present invention
The composition of water-soluble alcohol acid coating and operating process are as follows：
Composition：Water soluble alkyd resin 25%, iron oxide red 12%, barium carbonate 10%, 800 mesh coarse whitings are about
25%, dispersant 0.2%, anti-settling agent 0.5%, drier 0.45%, water (deionization) 22~25%, cosolvent 6%, drying aid
0.05%, ammonium hydroxide tune PH=7.5~9.
Process for preparation：It carries out ahead of schedule and water soluble alkyd resin and water is added stirs evenly with ammonium hydroxide tune PH=8~9, it is fully transparent
After be added iron oxide red, barium sulfate, coarse whiting, dispersant, anti-settling agent, drying aid are added when being distributed to fineness≤30 μm into machine and urge
Dry agent (common oiliness composite dry material) is finally surveyed after pH value reaches requirement and is packed.
It is shown in Table 2 from solid carbon dioxide dissolubility alkyd paint and the comparison of solvent based coating technical indicator.
Table 2 is compared from solid carbon dioxide dissolubility alkyd paint and solvent based coating technical indicator
Table 2 can be seen that：
A, in terms of dryness：The rate of drying of the ratio solvent-borne alkyd resins of water soluble alkyd resin is many soon, this is client
Most it is ready the product received.
B, in terms of hardness：Water soluble alkyd resin is more much higher than solvent-borne alkyd resins, is equivalent to polyurethane or amino is roasting
The hardness of paint, market are most ready to receive.
C, in terms of gloss：Its paint film is more slightly higher than solvent type, close to mixed paint gloss.
D, VOC (organic volatile) is nearly 3 times lower than solvent type, and the 20~40% of paint amount can also be added in use
Water, opposite VOC is lower, more environmentally friendly.
E, other：The same solvent type of water resistance, the same solvent type of anti-flash rusting, have preferably protectiveness, amount of water than lotion antirust
More.
In summary：Water solubility is than the antirust paint of solvent-borne alkyd resins with apparent dryness is fast, gloss is high, hardness
Greatly, the low feature of organic volatile has better performance than solvent type.
By quality versus, the present invention has better performance from solid carbon dioxide dissolubility alkyd paint than solvent based coating, so
Solvent type can be substituted completely, and cost is suitable or relatively low, there is better market prospects and economic benefit and society to imitate
Benefit.
Fatty acid methyl Lipase absobed of the present invention from the method for dry water soluble alkyd resin prepare from dry water soluble alkyd resin
And its coating, there is the features such as at low cost, dryness is fast, hardness is big, gloss is big, anti-flash rusting, water-fast, greatly reducing volatility has
Machine compound emission (VOC≤14%) accomplishes that solvent-borne alkyd resins truly are converted to water soluble paint.
Specific implementation mode
With reference to specific embodiment to the method for fatty acid methyl Lipase absobed from dry water soluble alkyd resin of the present invention make into
One step is described in detail.
Embodiment 1
Fatty acid methyl Lipase absobed of the present invention utilizes the aliphatic acid of waste grease production from the method for dry water soluble alkyd resin
Methyl esters is Material synthesis from dry water soluble alkyd resin, supplementary material by mass percentage fatty acid methyl ester 30%, linoleic acid 4%,
It is pentaerythrite 8%, ethylene glycol 6%, terephthalic acid (TPA) 16.4%, benzoic acid 3%, trimellitic anhydride 8%, organotin 0.8 ‰, ripe
The proportioning preparation of lime 0.15 ‰, triethylamine 4%, propandiol butyl ether 20.505%；Steps are as follows for synthetic operation：
(1) fatty acid methyl ester is added into reaction kettle, white lime is added after being preheating to 120~160 DEG C and continues to heat；
(2) pentaerythrite is added when being warming up to 180~200 DEG C, continues to heat up；
(3) when heat preservation 1~2 is small after temperature reaches 230~240 DEG C, linoleic acid is added after no methanol steams, to benzene two
Formic acid, ethylene glycol, benzoic acid and organotin are kept the temperature at a temperature of 220~240 DEG C；
(4) start to cool down when being reacted to acid value less than 6, trimellitic anhydride is added when temperature is down to 180 DEG C, in
Heat preservation to acid value is 36~42 at a temperature of 168~174 DEG C, viscosity is format (7：3) continue to cool down after 20~30s/25 DEG C；
(5) triethylamine and propandiol butyl ether are successively added after temperature is down to 100 DEG C or less, filtering is spare, and filtrate is
From dry water soluble alkyd resin.
Embodiment 2
Fatty acid methyl Lipase absobed of the present invention utilizes the aliphatic acid of waste grease production from the method for dry water soluble alkyd resin
Methyl esters is Material synthesis from dry water soluble alkyd resin, supplementary material by mass percentage fatty acid methyl ester 21%, linoleic acid 6%,
Pentaerythrite 9%, ethylene glycol 7%, terephthalic acid (TPA) 17%, benzoic acid 4%, trimellitic anhydride 9%, organotin 1.4 ‰, ripe stone
The proportioning preparation of ash 0.2 ‰, triethylamine 5%, propandiol butyl ether 21.84%；Synthetic operation step is the same as embodiment 1.
Embodiment 3
Fatty acid methyl Lipase absobed of the present invention utilizes the aliphatic acid of waste grease production from the method for dry water soluble alkyd resin
Methyl esters is Material synthesis from dry water soluble alkyd resin, supplementary material by mass percentage fatty acid methyl ester 36%, linoleic acid 4%,
Pentaerythrite 7%, ethylene glycol 5%, terephthalic acid (TPA) 15%, benzoic acid 2%, trimellitic anhydride 7%, organotin 0.7 ‰, ripe stone
The proportioning preparation of ash 0.12 ‰, triethylamine 3%, propandiol butyl ether 20.918%；Synthetic operation step is the same as embodiment 1.
Three above embodiment is prepared using same operating procedure from dry water soluble alkyd resin, with same iron oxide red anticorrosive paint
Formula prepares coating, is examined by national standard system, testing result comparison such as table 3.
3 each embodiment of table from dry water-soluble alcohol acid iron oxide red anticorrosive paint technical indicator contrast table
| Performance indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Surface drying, h | ≤0.5 | 1 | ≤0.5 |
| It does solid work, h | ≤5 | 8 | ≤5 |
| Hardness for 24 hours | 2H | HB~H | 2H |
| Gloss, % | 60~80 | 70~85 | 50~60 |
| Water resistance | ≥96 | ≥96 | ≤48 |
| PH value | 8~9 | 8~9 | 8~9 |
The product dryness that can be seen that embodiment 2 from the test result of table 3 is slack-off, and difference of hardness, gloss is got higher；Embodiment 3
Product gloss decline, water resistance be deteriorated；Coating comprehensive performance made from embodiment 1 is best, and embodiment 1 is most preferred embodiment.
Claims (1)
1. a kind of fatty acid methyl Lipase absobed is from the method for dry water soluble alkyd resin, the fatty acid methyl ester produced using waste grease
It is Material synthesis from dry water soluble alkyd resin, it is characterized in that：Supplementary material fatty acid methyl ester 21~36%, sub- by mass percentage
Oleic acid 4~6%, pentaerythrite 7~9%, ethylene glycol 5~7%, terephthalic acid (TPA) 15~17%, benzoic acid 2~4%, inclined benzene three
Acid anhydrides 7~9%, organotin 0.7~1.4 ‰, white lime 0.12~0.2 ‰, triethylamine 3~5%, propandiol butyl ether 20~22%
Proportioning prepare；Steps are as follows for synthetic operation：
(1) fatty acid methyl ester is added into reaction kettle, white lime is added after being preheating to 120~160 DEG C and continues to heat；
(2) pentaerythrite is added when being warming up to 180~200 DEG C, continues to heat up；
(3) when heat preservation 1~2 is small after temperature reaches 230~240 DEG C, linoleic acid, terephthaldehyde are added after no methanol steams
Acid, ethylene glycol, benzoic acid and organotin are kept the temperature at a temperature of 220~240 DEG C；
(4) start to cool down when being reacted to acid value less than 6, trimellitic anhydride is added when temperature is down to 180 DEG C, in 168~
Heat preservation to acid value is 36~42, format 7 at a temperature of 174 DEG C：3 viscosity continues to cool down after being 20~30s/25 DEG C；
(5) triethylamine and propandiol butyl ether are successively added after temperature is down to 100 DEG C or less, filtering is spare, and filtrate is from dry
Water soluble alkyd resin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611186281.XA CN106589334B (en) | 2016-12-20 | 2016-12-20 | Method of the fatty acid methyl Lipase absobed from dry water soluble alkyd resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611186281.XA CN106589334B (en) | 2016-12-20 | 2016-12-20 | Method of the fatty acid methyl Lipase absobed from dry water soluble alkyd resin |
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| CN106589334A CN106589334A (en) | 2017-04-26 |
| CN106589334B true CN106589334B (en) | 2018-07-24 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448269A (en) * | 2014-11-21 | 2015-03-25 | 无锡市虎皇漆业有限公司 | Quick-dried alkyd resin and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104448269A (en) * | 2014-11-21 | 2015-03-25 | 无锡市虎皇漆业有限公司 | Quick-dried alkyd resin and preparation method thereof |
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