CN117659366A - High-flash-point anti-undercut alkyd resin and preparation method thereof - Google Patents
High-flash-point anti-undercut alkyd resin and preparation method thereof Download PDFInfo
- Publication number
- CN117659366A CN117659366A CN202311586434.XA CN202311586434A CN117659366A CN 117659366 A CN117659366 A CN 117659366A CN 202311586434 A CN202311586434 A CN 202311586434A CN 117659366 A CN117659366 A CN 117659366A
- Authority
- CN
- China
- Prior art keywords
- parts
- acid
- alkyd resin
- solvent oil
- reflux
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920000180 alkyd Polymers 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 50
- 238000010992 reflux Methods 0.000 claims abstract description 31
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 16
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 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 claims abstract description 16
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 15
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000005642 Oleic acid Substances 0.000 claims abstract description 15
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 15
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 11
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940059574 pentaerithrityl Drugs 0.000 claims abstract description 11
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 20
- 229920005989 resin Polymers 0.000 claims description 18
- 239000011347 resin Substances 0.000 claims description 18
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 16
- 229930195729 fatty acid Natural products 0.000 claims description 16
- 239000000194 fatty acid Substances 0.000 claims description 16
- 150000004665 fatty acids Chemical class 0.000 claims description 16
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 12
- 229910052740 iodine Inorganic materials 0.000 claims description 12
- 239000011630 iodine Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 9
- 230000000573 anti-seizure effect Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 230000032050 esterification Effects 0.000 claims description 6
- 238000005886 esterification reaction Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- ADHNUPOJJCKWRT-JLXBFWJWSA-N (2e,4e)-octadeca-2,4-dienoic acid Chemical compound CCCCCCCCCCCCC\C=C\C=C\C(O)=O ADHNUPOJJCKWRT-JLXBFWJWSA-N 0.000 claims description 4
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 4
- LKOVPWSSZFDYPG-WUKNDPDISA-N trans-octadec-2-enoic acid Chemical compound CCCCCCCCCCCCCCC\C=C\C(O)=O LKOVPWSSZFDYPG-WUKNDPDISA-N 0.000 claims description 4
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000013557 residual solvent Substances 0.000 claims description 3
- 125000005842 heteroatom Chemical group 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 2
- 238000009835 boiling Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000003973 paint Substances 0.000 abstract description 12
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000035939 shock Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 27
- 235000019198 oils Nutrition 0.000 description 27
- 238000001035 drying Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 7
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 6
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 6
- 150000004671 saturated fatty acids Chemical class 0.000 description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 5
- 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 5
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 5
- 229960004488 linolenic acid Drugs 0.000 description 5
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 4
- 235000020778 linoleic acid Nutrition 0.000 description 4
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 4
- 235000021314 Palmitic acid Nutrition 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 235000012424 soybean oil Nutrition 0.000 description 3
- 239000003549 soybean oil Substances 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- RQFLGKYCYMMRMC-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O RQFLGKYCYMMRMC-UHFFFAOYSA-N 0.000 description 2
- ZUUFLXSNVWQOJW-MBIXAETLSA-N (2e,4e,6e)-octadeca-2,4,6-trienoic acid Chemical compound CCCCCCCCCCC\C=C\C=C\C=C\C(O)=O ZUUFLXSNVWQOJW-MBIXAETLSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention discloses a high-flash-point anti-biting alkyd resin and a preparation method thereof, wherein the alkyd resin is prepared from, by mass, 210-230 parts of oleic acid, 95-100 parts of monopentaerythritol, 110-120 parts of phthalic anhydride, 33-37 parts of rosin, 4-6 parts of a color reducer, 18-23 parts of reflux 100# solvent oil and 260-280 parts of 1500# solvent oil. The invention screens out various reaction raw material compositions and specific reaction process steps through a large number of experiments, the prepared alkyd resin has a flash point of more than 60 ℃ (closed), belongs to a class of chemicals, and the prepared paint is recoated without biting, has excellent glossiness, flexibility, shock resistance and hardness, and achieves good technical progress.
Description
Technical Field
The invention relates to high-flash-point anti-biting alkyd resin and a preparation method thereof.
Background
The common self-drying alkyd resin is prepared into varnish, ready-mixed paint, enamel and the like by adding a drier and automatically oxidizing and drying unsaturated bonds in fatty acid in air to form a film. The resin has the advantages of convenient construction, lower cost and good gloss, and is widely applied to the fields of steel structures, ships, trucks and the like for coating, and the general oil length of the resin is between 50 and 65. The surface is generally dried for 2-3 hours and the real drying is performed for 13-15 hours.
The alkyd resin is generally blended with dimethylbenzene and 200# solvent, the flash point of the resin is below 28 ℃ (closed), and the alkyd resin belongs to class A dangerous goods and brings inconvenience to storage and transportation. Along with the gradual emphasis of the national security and environmental protection work, the 1500# with high flash point is commonly used for replacing the 200# as the solvent of the self-drying alkyd resin in the industry of recent 4-5 years, so that the flash point of the resin is more than 60 ℃ (closed), belongs to the class-C chemicals, is convenient to store and transport, and relieves the pressure of the security work of enterprises.
Alkyd resins using 1500# solvent oil present new problems:
1,1500 # solvent oil has a flash point of between 63-70 ℃ (closed) and if the solvent is refluxed to remove a portion of the xylene at a later stage, otherwise the resin may have a flash point of between 55-60 ℃ and the resin flash point is unacceptable.
The evaporation rate of 2,1500 # solvent oil was slower than that of 200# solvent oil, and the drying property of the resin was deteriorated.
The main component of 3,1500 # solvent oil is aromatic hydrocarbon, and the main component of 200# solvent oil is aliphatic hydrocarbon, the former is more soluble in paint film than the latter. In the actual coating process, secondary spraying is needed in many occasions, so that the problems of biting, wrinkling, stripping and the like of the lower coating by the upper paint film can be caused.
In summary, although the existing self-drying resin blended with 1500# alkene can achieve a flash point of more than 60 ℃, improvement in the stability of the flash point, the dryness of the resin and particularly the anti-seizure performance is still needed.
Disclosure of Invention
The invention aims to: the invention aims to provide self-drying alkyd resin which has high flash point, is unaffected in dryness, has the flash point stabilized above 60 ℃ and is resistant to biting; it is another object of the present invention to provide a process for its preparation.
The technical scheme is as follows: in order to achieve the above purpose, the invention adopts the following technical scheme:
the high-flash-point anti-biting alkyd resin is prepared from the following raw materials in parts by weight:
210-230 parts of oleic acid, 95-100 parts of monopentaerythritol, 110-120 parts of phthalic anhydride, 33-37 parts of rosin, 4-6 parts of color reducer, 18-23 parts of reflux 100# solvent oil and 260-280 parts of 1500# solvent oil raw materials.
As a preferred embodiment, the quick-drying high-performance alkyd resin comprises oleic acid which is a fatty acid of octadeca (typically OA-7075 of Fengyi Fine chemistry Co., ltd.), wherein the content of octadecenoic acid is not less than 75%, the content of octadecadienoic acid is not more than 13%, the content of stearic acid is not more than 12%, the content of other hetero acids is not more than 1%, and the iodine value is 88-96g I 2 Between 100g and between 195 and 205 mgKOH/g.
As a preferable scheme, the high-flash-point anti-biting alkyd resin is rosin with an acid value of 165-175mgKOH/g and a softening point of more than 76 ℃.
As a preferable scheme, the high-flash-point anti-biting alkyd resin is characterized in that the color reducer is at least one or a mixture of hypophosphorous acid and triphenyl phosphite.
As a preferable scheme, the high-flash-point anti-biting alkyd resin is characterized in that 100# solvent oil is a solvent with a distillation range of 155-175 ℃ and a density of 0.862-0.875 (20 ℃).
As a preferable scheme, the high-flash-point anti-biting alkyd resin is characterized in that the 1500# solvent oil is a solvent with a distillation range of 180-210 ℃ and a density of 0.900-0.930 (20 ℃), and the flash point is 63-70 ℃ (closed).
The invention relates to a preparation method of high-flash-point anti-biting alkyd resin, which comprises the following steps:
1) After introducing nitrogen into a reaction kettle for 15 minutes, adding 210-230 parts by weight of oleic acid, 95-100 parts by weight of monopentaerythritol, 110-120 parts by weight of phthalic anhydride, 33-37 parts by weight of rosin, 4-6 parts by weight of color reducer and 18-23 parts by weight of reflux 100# solvent oil into the reaction kettle, heating to reflux nitrogen, continuously heating to 180-190 ℃ for 2 hours, heating to 190-200 ℃ for 2 hours, heating to 210-230 ℃ for reflux esterification, and starting sampling to measure acid value and viscosity after refluxing for 1 hour;
2) Until an acid value of less than 20mgKOH/g is reached, viscosity: 17-22 seconds format pipe (1500 # is blended with 60 solid content), the temperature is reduced immediately after the acid value and the viscosity are qualified, when the kettle temperature is reduced to 200 ℃, the 1500# solvent oil is partially diluted, the diluted kettle is turned over, other residual solvents are pumped into the diluted kettle, and the temperature is reduced to below 100 ℃ to obtain the resin with 59-61% of solid content.
The invention mainly improves the defects of the existing high-flash alkyd resin through the following schemes:
1. the invention discovers that the dryness of the self-drying alkyd resin is related to the iodine value of the used fatty acid and the content of saturated fatty acid in the fatty acid, and the higher the content of saturated fatty acid is, the slower the dryness is, in the prior art, the self-drying alkyd resin generally uses fatty acid with the iodine value of 130-135, mainly from soybean oil, the hexadecanoic acid accounts for 10-12%, the octadecanoic acid (stearic acid) accounts for 4-5%, and the total content of saturated fatty acid accounts for about 15%. The oleic acid adopted by the invention (typically OA-7075 of Fengyi Fine chemistry Co., ltd.) has a stearic acid content of not more than 12%, although the iodine value is only 88-96g I2/100g, the saturated fatty acid is lower than the common fatty acid with an iodine value of 130-135, so that the dryness is not inferior to the fatty acid with the iodine value of 130-135, the flash point is stabilized above 60 ℃, and the anti-biting performance of the prepared paint is more outstanding.
2. The invention also finds that the anti-seizure property of the self-drying alkyd resin is mainly related to the content of octadecadienoic acid (hereinafter referred to as linoleic acid) and octadecatrienoic acid (hereinafter referred to as linolenic acid) in the used fatty acid, and the higher the content is, the worse the anti-seizure property is, in particular the content of linolenic acid. The content of the fatty acid with iodine value of 130-135, linoleic acid is about 50%, the content of linolenic acid is 7-9%, and the total content of linoleic acid and linolenic acid is about 58%. The oleic acid adopted by the invention has the content of octadecenoic acid not lower than 75%, the content of octadecadienoic acid (linoleic acid) not higher than 13%, the content of stearic acid not higher than 12%, and no linolenic acid, and the anti-biting performance is obviously improved compared with the common fatty acid with the iodine value of 130-135.
3. The rosin accounting for 8% of the formula is used, so that the dryness of the resin is improved, and part of oleic acid is replaced, so that the undercut of the resin is reduced by 48% of the formula.
4. According to the invention, 100# solvent oil is used as a reflux solvent instead of common xylene, because the flash point (42-47 ℃) of the 100# solvent oil is higher than that (17-25 ℃) of the xylene, the reflux solvent does not need to be removed in the later stage, the flash point of the alkyd resin is stabilized between 61-65 ℃, and the reject ratio is reduced. And the distillation range of the 100# solvent oil is 155-175 ℃, and the normal reaction temperature is 210-230 ℃, so that the reflux dehydration effect is less.
The beneficial effects are that: compared with the prior art, the invention has the following advantages:
according to the invention, various reaction raw materials are screened out through a large number of experiments, and the high-flash-point anti-biting alkyd resin prepared under specific technological conditions by adopting specific oleic acid, monopentaerythritol, phthalic anhydride, rosin, 100# solvent oil and 1500# solvent oil has the advantages of high flash point, over 60 ℃, no influence on dryness, excellent anti-biting performance, excellent glossiness, flexibility, impact resistance and hardness, and good technical progress.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Embodiments of the present invention will be described in detail with reference to examples, which are not to be construed as specific conditions, either as normal conditions or as recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The 100# solvent naphtha described in the examples below is a solvent having a distillation range of 155-175 c and a density of 0.862-0.875 at 20 c. The 1500# solvent oil is a solvent with the distillation range of 180-210 ℃, the density of 20 ℃ of 0.900-0.930 and the flash point of 63-70 ℃.
The compositions of the raw materials in the following examples are shown in Table 1:
table 1 raw material composition of each example
The preparation method of the quick-drying high-performance alkyd resin comprises the following steps:
1) Introducing nitrogen into a reaction kettle for 15 minutes, adding oleic acid, monopentaerythritol, phthalic anhydride, rosin, a color reducing agent and reflux 100# solvent oil into the reaction kettle according to the mass parts of the above examples, heating to reflux nitrogen, continuously heating to 180-190 ℃ for 2 hours, heating to 190-200 ℃ for 2 hours, heating to 210-230 ℃ for reflux esterification after 2 hours, and starting sampling to measure acid value and viscosity after 1 hour of reflux;
2) Until an acid value of less than 20mgKOH/g is reached, viscosity: 17-22 seconds format pipe (1500 # is blended with 60 solid content), and immediately cooling after the acid value and viscosity are qualified, when the kettle temperature is reduced to 200 ℃, diluting part of 15% of 1500# solvent oil, turning into a diluting kettle, pumping the rest 85% of 1500# solvent oil into the diluting kettle, and cooling to below 100 ℃ to obtain resin with 59-61% of solid content.
Comparative example 1
After introducing nitrogen into a reaction kettle for 15 minutes, adding 220 parts by mass of fatty acid with an iodine value of 133 (mainly from soybean oil, 10-12% of hexadecanoic acid, 4-5% of stearic acid and about 15% of total saturated fatty acid), 98 parts of monopentaerythritol, 115 parts of phthalic anhydride, 35 parts of rosin, 5 parts of hypophosphorous acid and 22 parts of reflux 100# solvent oil into the reaction kettle, heating to reflux nitrogen, continuously heating to 180-190 ℃, preserving heat for 2 hours, heating to 190-200 ℃, preserving heat for 2 hours, heating to 210-230 ℃ for reflux esterification for 2 hours, and starting sampling to measure acid value and viscosity after reflux for 1 hour; until an acid value of less than 20mgKOH/g is reached, viscosity: 17-22 seconds format tube (1500 # is blended with 60 solid content), the temperature is reduced immediately after the acid value and the viscosity are qualified, and when the kettle temperature is reduced to 200 ℃, 276 parts by mass of 1500# solvent oil is diluted and reduced to below 100 ℃ to obtain the resin of comparative example 1 with 59.6% solid content.
Comparative example 2
After introducing nitrogen into a reaction kettle for 15 minutes, adding 253 parts by mass of fatty acid with an iodine value of 133 (mainly from soybean oil, 10-12% of hexadecanoic acid, 4-5% of octadecanoic acid (stearic acid) and about 15% of total saturated fatty acid content), 102 parts of monopentaerythritol, 124 parts of phthalic anhydride, 5 parts of hypophosphorous acid and 22 parts of reflux 100# solvent oil into the reaction kettle, heating to reflux nitrogen, continuously heating to 180-190 ℃, preserving heat for 2 hours, heating to 190-200 ℃, preserving heat for 2 hours, heating to 210-230 ℃ for reflux esterification for 2 hours, and starting sampling to measure acid value and viscosity after refluxing for 1 hour; until an acid value of less than 20mgKOH/g is reached, viscosity: 17-22 seconds format tube (1500 # is blended with 60 solid content), the temperature is reduced immediately after the acid value and the viscosity are qualified, and when the kettle temperature is reduced to 200 ℃, 276 parts by mass of 1500# solvent oil is diluted and reduced to below 100 ℃ to obtain the resin of comparative example 2 with the solid content of 60.1%.
TABLE 2 resin flash point
Application example 1
1. Alkyd resins obtained in the above examples 1 to 5 are prepared into colored paint according to the following formula of the colored paint shown in table 3:
TABLE 3 color paint formulation
2. Color paint detection
The following tests were carried out on the colored paints (dispersion grinding) prepared in examples 1 to 5 and comparative examples 1 to 2 above:
wherein the flexibility is in accordance with GB/T1731-2020 standard method.
Impact strength is in accordance with GB/T1732-2020 standard.
The surface drying and the real drying are according to the GB/T1728-2020 standard method.
Gloss is in accordance with GB/T9754-2007 standard method.
The specific paint test results are shown in table 4:
TABLE 4 color paint test results
The experimental results show that the self-drying alkyd resin prepared by adopting the compatibility of the fatty acid with octadeca (typically oleic acid with the content of octadecenoic acid not lower than 75% of OA-7075 of Fengyi fine chemical Co., ltd.), rosin and No. 100 solvent oil has high flash point, is not influenced in dryness, is stable at the temperature of more than 60 ℃ and has more outstanding anti-biting performance compared with the fatty acid with iodine value of 133 adopted in comparative documents 1 and 2. It can be seen from comparative examples 1 and 2 that the anti-seizure properties after recoating are better after addition of the rosin component.
The experimental result shows that the invention can overcome the defects of the prior art and obtain good technical effect.
Claims (9)
1. A high flash point anti-biting alkyd resin is characterized in that: the composite material is prepared from the following raw materials in parts by weight:
oleic acid, monopentaerythritol, phthalic anhydride, rosin, a color reducing agent, refluxing 100# solvent oil and 1500# solvent oil.
2. The high flash point anti-seizure alkyd resin of claim 1, wherein: the composite material is prepared from the following raw materials in parts by weight:
210-230 parts of oleic acid, 95-100 parts of monopentaerythritol, 110-120 parts of phthalic anhydride, 33-37 parts of rosin, 4-6 parts of color reducer, 18-23 parts of reflux 100# solvent oil and 260-280 parts of 1500# solvent oil.
3. The high flash point anti-biting alkyd resin of claim 1, wherein the oleic acid is a fatty acid of octadeca, wherein the fatty acid of octadeca has an octadecenoic acid content of not less than 75%, an octadecadienoic acid content of not more than 13%, a stearic acid content of not more than 12%, other hetero acids content of not more than 1%, and an iodine value of 88-96g I 2 The acid value is 195-205 mgKOH/g.
4. The high flash point anti-biting alkyd resin of claim 1, wherein the rosin is a rosin having an acid number between 165 and 175mgKOH/g and a softening point greater than 76 ℃.
5. The high flash point anti-seizure alkyd resin of claim 1, wherein the color reducing agent is at least one of hypophosphorous acid and triphenyl phosphite or a mixture thereof.
6. The high flash point anti-seizure alkyd resin as recited in claim 1, wherein said 100# solvent oil is a solvent having a boiling range of 155-175 ℃ and a 20 ℃ density of between 0.862-0.875.
7. The high flash point anti-seizure alkyd resin as recited in claim 1, wherein the 1500# solvent oil is a solvent having a distillation range of 180-210 ℃, a density of 20 ℃ of 0.900-0.930, and a flash point of 63-70 ℃.
8. The method for preparing the high-flash-point anti-biting alkyd resin as defined in any one of claims 1 to 7, which is characterized by comprising the following steps:
1) After introducing nitrogen into a reaction kettle, adding oleic acid, monopentaerythritol, phthalic anhydride, rosin, a color reducing agent and reflux 100# solvent oil into the reaction kettle, heating to reflux, guan Danqi, continuously heating to 180-190 ℃ for 1-2 hours, heating to 190-200 ℃ for 1-2 hours, heating to 210-230 ℃ for reflux esterification after 1-2 hours, and starting sampling to measure acid value and viscosity after reflux;
2) And immediately cooling until the acid value and the viscosity are qualified, diluting the 1500# solvent oil part when the kettle temperature is reduced to 200-210 ℃, turning over the diluted kettle, pumping other residual solvents into the diluted kettle, and cooling to below 100 ℃ to obtain the resin.
9. The method for preparing the high-flash-point anti-biting alkyd resin, as claimed in claim 8, comprising the following steps:
1) Introducing nitrogen into a reaction kettle for 15 minutes, adding 210-230 parts by weight of oleic acid, 95-100 parts by weight of monopentaerythritol, 110-120 parts by weight of phthalic anhydride, 33-37 parts by weight of rosin, 4-6 parts by weight of color reducer and 18-23 parts by weight of reflux 100# solvent oil into the reaction kettle, heating to reflux, guan Danqi, continuously heating to 180-190 ℃ for 2 hours, heating to 190-200 ℃ for 2 hours, heating to 210-230 ℃ for reflux esterification again for 2 hours, and starting sampling to measure acid value and viscosity after reflux for 1 hour;
2) Until an acid value of less than 20mgKOH/g is reached, viscosity: and (3) carrying out 17-22 seconds format pipe/1500 # mixing 60 solid content, immediately cooling after the acid value and viscosity are qualified, diluting the 1500# solvent oil part when the kettle temperature is reduced to 200 ℃, turning over the diluted kettle, pumping other residual solvents into the diluted kettle, and cooling to below 100 ℃ to obtain the resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311586434.XA CN117659366A (en) | 2023-11-27 | 2023-11-27 | High-flash-point anti-undercut alkyd resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311586434.XA CN117659366A (en) | 2023-11-27 | 2023-11-27 | High-flash-point anti-undercut alkyd resin and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117659366A true CN117659366A (en) | 2024-03-08 |
Family
ID=90076286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311586434.XA Pending CN117659366A (en) | 2023-11-27 | 2023-11-27 | High-flash-point anti-undercut alkyd resin and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117659366A (en) |
-
2023
- 2023-11-27 CN CN202311586434.XA patent/CN117659366A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100526362C (en) | Water-soluble alcohol-acid resin solution and water-soluble alcohol-acid amino baking paint and preparing method | |
| US20110230616A1 (en) | Water reducible alkyd resins | |
| CN108373760A (en) | A kind of water-based acrylic acid modified alcoholic acid antirust paint and preparation method thereof | |
| CN111607285B (en) | Solvent-free metal printing ink and preparation method and application thereof | |
| DE1900464A1 (en) | Process for the modification of alkyd resins for greasy, oily printing inks | |
| CN112812664A (en) | Water-based quick-drying low-VOC alkyd paint and preparation method thereof | |
| CN111944133B (en) | Quick-drying high-performance alkyd resin and preparation method thereof | |
| CN114773970A (en) | Water-based high-volume solid-content steel structure normal-temperature anticorrosive paint and preparation method thereof | |
| CN110092895B (en) | Air-drying waterborne alkyd resin and preparation method thereof | |
| CN117659366A (en) | High-flash-point anti-undercut alkyd resin and preparation method thereof | |
| US6355722B2 (en) | Aqueous binder solutions and dispersions | |
| CN114479625A (en) | High-flash-point alkyd resin protective finish | |
| CN114316748B (en) | High-corrosion-resistance thick-paste type water-based paint, and preparation method and application method thereof | |
| CN112126024B (en) | Quick-drying water-based modified oil and preparation method thereof | |
| CN113136025B (en) | Water-soluble saturated polyester resin suitable for water-based steel drum coating and preparation method thereof | |
| FI110689B (en) | Resin mixture containing an alkyd resin and a reactive diluent | |
| US3779961A (en) | Lacquer binders | |
| DE2403212C3 (en) | Process for the preparation of a resin for printing inks | |
| CN112980323B (en) | Anti-yellowing composition for duct gloss oil, anti-yellowing environment-friendly duct gloss oil and preparation method thereof | |
| CN108440746B (en) | Low-chain active resin modified alkyd resin, preparation method and self-drying paint | |
| CN107778468A (en) | Quick-dry type medium oil alkyd and preparation method thereof and quick-dry type varnish | |
| US2087395A (en) | Liquid coating composition | |
| CN115677991A (en) | Water-based alkyd resin with high solid content and high flash point baking varnish and preparation method thereof | |
| CN111154082A (en) | One-step method for preparing quick-drying water-based alkyd resin and preparation method thereof | |
| DE2618629A1 (en) | MODIFIED AIR-DRYING ALKYD RESINS |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |