CN110616005A - High-iron putty and preparation method thereof - Google Patents
High-iron putty and preparation method thereof Download PDFInfo
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- CN110616005A CN110616005A CN201911073693.6A CN201911073693A CN110616005A CN 110616005 A CN110616005 A CN 110616005A CN 201911073693 A CN201911073693 A CN 201911073693A CN 110616005 A CN110616005 A CN 110616005A
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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
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/676—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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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
- C08G63/78—Preparation processes
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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
- C09D5/34—Filling pastes
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Macromonomer-Based Addition Polymer (AREA)
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Abstract
The invention belongs to the field of coatings, and particularly relates to high-iron putty which comprises a component A and a component B, wherein the component A comprises the following components in percentage by weight: 34-38% of polyester resin; 0.4 to 0.8 percent of dispersant; 0.06 to 0.1 percent of stabilizer; 3-5% of a diluent; the balance of filler. The main innovation point of the putty is the compound use of the trihydric alcohol and the dihydric alcohol, and simultaneously, under the action of the maleic anhydride, the tetrahydrophthalic anhydride and preferably the air-drying monomer trimethylolpropane diallyl ether, the putty can show better flexibility and adhesive force, and the application performance on high-speed rails is improved. Meanwhile, in the prior art, the linoleic acid is an excellent putty modifier, and the impact resistance of the high-iron putty can be improved by matching with the saturated fatty acid myristic acid.
Description
Technical Field
The invention relates to the field of coatings, in particular to high-iron putty and a preparation method thereof.
Background
CN201611016419.1 discloses a light multifunctional putty and a preparation method thereof, wherein the light multifunctional putty comprises the following components in parts by mass: 30-50 parts of unsaturated resin, 2-6 parts of styrene, 1-2.6 parts of auxiliary agent, 2-8 parts of pigment, 0.5-1.5 parts of accelerator and 38-70 parts of powder; the accelerator is a cobalt salt accelerator, and the pigment is titanium dioxide.
It is knife coating type putty, the flexibility is about 50mm, and the adhesive force is 5-6 MPa.
The company now develops an atomic ash suitable for high-speed rail.
Based on the characteristics of high-frequency and high-speed moving carriers of high-speed rails, the putty is required to show excellent adhesive force and flexibility, so that the coating can be kept stable on a locomotive moving at high speed, and the service life is prolonged. Meanwhile, the quick drying property of the concrete needs to be kept, so that the construction effect is improved.
The technical problem that this application will solve is: provides a high-iron putty which is used for solving the problems of poor adhesive force and poor flexibility of the traditional putty.
Disclosure of Invention
The invention aims to provide high-iron putty, which has the main innovation point that the putty is compounded by using trihydric alcohol and dihydric alcohol, and can show better flexibility and adhesive force under the action of maleic anhydride, tetrahydrophthalic anhydride and preferably air-drying monomer trimethylolpropane diallyl ether, so that the application performance of the high-iron putty on high-iron is improved. Meanwhile, in the prior art, the linoleic acid is an excellent putty modifier, and the impact resistance of the high-iron putty can be improved by matching with the saturated fatty acid myristic acid.
Unless otherwise specified, the percentages and parts in the present invention are in weight percent.
In order to achieve the purpose, the invention provides the following technical scheme:
the high-iron atomic ash comprises a component A and a component B, wherein the component A comprises the following components in percentage by weight:
34-38% of polyester resin; 0.4 to 0.8 percent of dispersant; 0.06 to 0.1 percent of stabilizer; 3-5% of a diluent; the balance of filler;
the component B is cyclohexanone peroxide;
the weight ratio of the component A to the component B is 100: 2;
the polyester resin is prepared by the following method:
step 1: mixing polybasic acid, polyalcohol and trimethylolpropane diallyl ether, and adding a polymerization inhibitor and an antioxidant;
step 2: esterifying and dehydrating for 1-2h at the temperature of 140 ℃ and 150 ℃;
and step 3: heating to 185-195 ℃, reacting at constant temperature for at least 3h, measuring the acid value, adding linoleic acid and myristic acid when the acid value is 90-100KOH/g, and cooling to 160-165 ℃;
and 4, step 4: heating to 185 ℃, keeping the temperature for at least 2h, measuring the acid value, and starting vacuum-pumping dehydration for 1.5-2h when the acid value is less than or equal to 70 KOH/g;
and 5: adding styrene for dilution, adding an antioxidant, reacting for 1-1.5h, and then cooling to 60-70 ℃;
the molar ratio of the polyhydric alcohol to the polybasic acid is 1-1.05: 1;
the polyol consists of diethylene glycol, 1, 4-cyclohexanedimethanol and glycerol in a weight ratio of 7:2: 1;
the polybasic acid consists of maleic anhydride, tetrahydrophthalic anhydride and isophthalic acid in a weight ratio of 6:3.2-3.5: 0.5-0.8;
the total amount of the linoleic acid and the myristic acid is 8-12% of the total weight of the polybasic acid and the polyhydric alcohol;
the styrene accounts for 30 to 35 percent of the total weight of the polybasic acid and the polyhydric alcohol;
10-15% trimethylolpropane diallyl ether relative to the total weight of the polyacid and the polyol.
In the high-iron atomic ash, the polymerization inhibitor is one or more of hydroquinone, NSI, I-95 and TBC, and the polymerization inhibitor is 0.01-0.03 percent of the total weight of polybasic acid and polyhydric alcohol;
the antioxidant used in the step 1 and the step 5 is organic phosphite ester or phenolic antioxidant, and the antioxidant accounts for 0.03-0.1% of the total weight of the polybasic acid and the polyhydric alcohol.
In the high-iron atomic ash, the diluent is styrene.
In the high-iron putty, the filler is talcum powder.
In the high-iron putty, the weight ratio of the linoleic acid to the myristic acid is 7-8: 2-3.
Meanwhile, the invention also discloses a preparation method of the high-iron atomic ash, which comprises the following steps:
step 1: mixing and dispersing polyester resin, a dispersing agent, a stabilizing agent and a diluting agent;
step 2: adding the filler and continuously dispersing for 0.5-1 h;
and step 3: vacuumizing for 15-30min to obtain the component A.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the combination of the trihydric alcohol and the dihydric alcohol, and simultaneously can show better flexibility and adhesive force under the action of maleic anhydride, tetrahydrophthalic anhydride and preferably air-drying monomer trimethylolpropane diallyl ether, thereby improving the application performance on high-speed rails.
More specifically, the linoleic acid has air-drying property, and the trimethylolpropane diallyl ether also has air-drying property, and the combination of the linoleic acid and the trimethylolpropane diallyl ether can improve the air-drying speed of the whole formula. Meanwhile, the impact resistance can be improved by matching with the saturated fatty acid myristic acid.
Meanwhile, the invention also discloses the atomic ash and a preparation method thereof.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1 polyester preparation
A preparation method of polyester resin for high-iron putty comprises the following steps:
step 1: mixing polybasic acid, polyalcohol and trimethylolpropane diallyl ether, and adding a polymerization inhibitor and an antioxidant;
step 2: esterification and dehydration are carried out for 1.5h at the temperature of 140 ℃ and 150 ℃;
and step 3: heating to 190 ℃, reacting for 3h at constant temperature, measuring the acid value, adding linoleic acid and cooling to 160-165 ℃ when the acid value is 90-100 KOH/g;
and 4, step 4: heating to 180 ℃ and 185 ℃, preserving the temperature for 2h, measuring the acid value, and starting vacuum-pumping dehydration for 1.5-2h when the acid value is less than or equal to 70 KOH/g;
and 5: adding styrene for dilution, adding an antioxidant, reacting for 1-1.5h, and then cooling to 60-70 ℃;
the dosage of each formula is as follows:
diethylene glycol: 70g of a mixture; 1, 4-cyclohexanedimethanol: 20 g: glycerol: 10g of a mixture; maleic anhydride: 59.64 g; tetrahydrophthalic anhydride: 29.82 g; isophthalic acid: 9.94 g; linoleic acid: 15.95 g; myristic acid: 4g of the total weight of the mixture; styrene: 60.47g of trimethylolpropane diallyl ether, 19.94g of trimethylolpropane diallyl ether;
the polymerization inhibitor is hydroquinone, and the dosage is 0.02 g; the antioxidant is627AV, 0.1g in step 1; the dosage of the step 5 is 0.1 g.
Example 2 polyester preparation
A preparation method of polyester resin for high-iron putty comprises the following steps:
step 1: mixing polybasic acid, polyalcohol and trimethylolpropane diallyl ether, and adding a polymerization inhibitor and an antioxidant;
step 2: esterification and dehydration are carried out for 1.5h at the temperature of 140 ℃ and 150 ℃;
and step 3: heating to 190 ℃, reacting for 3h at constant temperature, measuring the acid value, adding linoleic acid and cooling to 160-165 ℃ when the acid value is 90-100 KOH/g;
and 4, step 4: heating to 180 ℃ and 185 ℃, preserving the temperature for 2h, measuring the acid value, and starting vacuum-pumping dehydration for 1.5-2h when the acid value is less than or equal to 70 KOH/g;
and 5: adding styrene for dilution, adding an antioxidant, reacting for 1-1.5h, and then cooling to 60-70 ℃;
the dosage of each formula is as follows:
diethylene glycol: 70g of a mixture; 1, 4-cyclohexanedimethanol: 20 g: glycerol: 10g of a mixture; maleic anhydride: 59.57 g; tetrahydrophthalic anhydride: 31.8 g; isophthalic acid: 8g of the total weight of the mixture; linoleic acid: 15.94 g; myristic acid: 3.99 g; styrene: 59.78 g; 29.89g of trimethylolpropane diallyl ether;
the polymerization inhibitor is hydroquinone, and the dosage is 0.02 g; the antioxidant is627AV, 0.1g in step 1; the dosage of the step 5 is 0.1 g.
Example 3 polyester preparation
A preparation method of polyester resin for high-iron putty comprises the following steps:
step 1: mixing polybasic acid, polyalcohol and trimethylolpropane diallyl ether, and adding a polymerization inhibitor and an antioxidant;
step 2: esterification and dehydration are carried out for 1.5h at the temperature of 140 ℃ and 150 ℃;
and step 3: heating to 190 ℃, reacting for 3h at constant temperature, measuring the acid value, adding linoleic acid and cooling to 160-165 ℃ when the acid value is 90-100 KOH/g;
and 4, step 4: heating to 180 ℃ and 185 ℃, preserving the temperature for 2h, measuring the acid value, and starting vacuum-pumping dehydration for 1.5-2h when the acid value is less than or equal to 70 KOH/g;
and 5: adding styrene for dilution, adding an antioxidant, reacting for 1-1.5h, and then cooling to 60-70 ℃;
the dosage of each formula is as follows:
diethylene glycol: 70g of a mixture; 1, 4-cyclohexanedimethanol: 20 g: glycerol: 10g of a mixture; maleic anhydride: 59.72 g; tetrahydrophthalic anhydride: 27.87 g; isophthalic acid: 11.94 g; linoleic acid: 13.97 g; myristic acid: 5.99 g; styrene: 69.83 g; 24g of trimethylolpropane diallyl ether;
the polymerization inhibitor is hydroquinone, and the dosage is 0.02 g; the antioxidant is627AV, 0.1g in step 1; the dosage of the step 5 is 0.1 g.
Example 4 high iron atomic Ash preparation
Step 1: mixing and dispersing the polyester resin prepared in the example 1, a dispersing agent, a stabilizing agent and a diluting agent;
step 2: adding the filler and continuously dispersing for 0.5-1 h;
and step 3: vacuumizing for 20 min.
The formula is as follows:
350g of polyester resin;
6g of a dispersant (ammonium salt dispersant for coating);
stabilizer (a)627AV)1g；
Diluent (styrene) 40g
603g of talcum powder.
Example 5 high iron putty preparation
Step 1: mixing and dispersing the polyester resin prepared in the example 2, a dispersing agent, an accelerating agent, a stabilizing agent and a diluting agent;
step 2: adding the filler and continuing to disperse for 0.5-1 h.
And step 3: vacuumizing for 20 min.
The formula is as follows:
380g of polyester resin;
8g of dispersing agent;
0.8g of stabilizer;
50g of diluent
561g of talcum powder.
Example 6 high iron putty preparation
Step 1: mixing and dispersing the polyester resin prepared in the example 3, a dispersing agent, an accelerating agent, a stabilizing agent and a diluting agent;
step 2: adding the filler and continuing to disperse for 0.5-1 h.
And step 3: vacuumizing for 20 min.
The formula is as follows:
340g of polyester resin;
4g of dispersing agent;
0.7g of stabilizer;
diluent 35g
620.3g of talcum powder.
Comparative example 1
The same as example 1 was true except that:
the polyol consists of diethylene glycol, 1, 4-cyclohexanedimethanol and triethylene glycol in a weight ratio of 7:2: 1;
the polybasic acid consists of maleic anhydride and tetrahydrophthalic anhydride in a weight ratio of 6: 4;
the linoleic acid is 10% of the total weight of the polybasic acid and the polyhydric alcohol;
the styrene is 35% by weight of the total weight of the polybasic acid and the polyhydric alcohol.
Atomic ash preparation reference example 4.
Comparative example 2
The same as example 1 was true except that:
the fatty acid was linoleic acid only, and the amount used was 20 g.
Atomic ash preparation reference example 4.
Comparative example 3
The same as example 1 was true except that:
the use of trimethylolpropane diallyl ether is eliminated.
Atomic ash preparation reference example 4.
Comparative example 4
The same as example 1 was true except that:
terephthalic acid is used instead of isophthalic acid.
Atomic ash preparation reference example 4.
Comparative example 5
The same as example 1 was true except that:
the isophthalic acid is replaced by phthalic acid.
Atomic ash preparation reference example 4.
The use method of the high-iron-content putty comprises the following steps:
the putty prepared in examples 4-6 and comparative example 1 was mixed with a curing agent at a ratio of 100:2 (by weight) and used according to the test method.
Performance testing
Test results, test methods are given in Table 1 below
TABLE 1
Through the tests, the compound use of the trihydric alcohol and the dihydric alcohol is found, and meanwhile, under the action of the maleic anhydride, the tetrahydrophthalic anhydride and preferably the air-drying monomer trimethylolpropane diallyl ether, the better flexibility and adhesive force can be shown, and the application performance on high-speed rails is improved.
More specifically, the linoleic acid has air-drying property, and the trimethylolpropane diallyl ether also has air-drying property, and the combination of the linoleic acid and the trimethylolpropane diallyl ether can improve the air-drying speed, the coating flexibility and the adhesion of the whole formula.
Linoleic acid is polyunsaturated fatty acid, and can improve the shock resistance by being matched with the myristic acid, which is a saturated fatty acid.
The contribution of phthalic acid to impact resistance is limited and the improvement in the overall performance of terephthalic acid is detrimental.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. The high-iron atomic ash is characterized by comprising a component A and a component B, wherein the component A comprises the following components in percentage by weight:
34-38% of polyester resin; 0.4 to 0.8 percent of dispersant; 0.06 to 0.1 percent of stabilizer; 3-5% of a diluent; the balance of filler;
the component B is cyclohexanone peroxide;
the weight ratio of the component A to the component B is 100: 2;
the polyester resin is prepared by the following method:
step 1: mixing polybasic acid, polyalcohol and trimethylolpropane diallyl ether, and adding a polymerization inhibitor and an antioxidant;
step 2: esterifying and dehydrating for 1-2h at the temperature of 140 ℃ and 150 ℃;
and step 3: heating to 185-195 ℃, reacting at constant temperature for at least 3h, measuring the acid value, adding linoleic acid and myristic acid when the acid value is 90-100KOH/g, and cooling to 160-165 ℃;
and 4, step 4: heating to 185 ℃, keeping the temperature for at least 2h, measuring the acid value, and starting vacuum-pumping dehydration for 1.5-2h when the acid value is less than or equal to 70 KOH/g;
and 5: adding styrene for dilution, adding an antioxidant, reacting for 1-1.5h, and then cooling to 60-70 ℃;
the molar ratio of the polyhydric alcohol to the polybasic acid is 1-1.05: 1;
the polyol consists of diethylene glycol, 1, 4-cyclohexanedimethanol and glycerol in a weight ratio of 7:2: 1;
the polybasic acid consists of maleic anhydride, tetrahydrophthalic anhydride and isophthalic acid in a weight ratio of 6:3.2-3.5: 0.5-0.8;
the total amount of the linoleic acid and the myristic acid is 8-12% of the total weight of the polybasic acid and the polyhydric alcohol;
the styrene accounts for 30 to 35 percent of the total weight of the polybasic acid and the polyhydric alcohol;
10-15% trimethylolpropane diallyl ether relative to the total weight of the polyacid and the polyol.
2. The high iron putty as set forth in claim 1 wherein the polymerization inhibitor is one or more of hydroquinone, NSI, I-95, TBC, and the polymerization inhibitor is 0.01-0.03% of the total weight of the polybasic acid and the polyhydric alcohol;
the antioxidant used in the step 1 and the step 5 is organic phosphite ester or phenolic antioxidant, and the antioxidant accounts for 0.03-0.1% of the total weight of the polybasic acid and the polyhydric alcohol.
3. The high iron putty as set forth in claim 1 wherein the diluent is styrene.
4. The high iron putty as set forth in claim 1 wherein the filler is talc.
5. The high iron putty as set forth in claim 1 wherein the weight ratio of linoleic acid to myristic acid is 7-8: 2-3.
6. A method for preparing the high iron putty as set forth in any one of claims 1 to 5, characterized by comprising the steps of:
step 1: mixing and dispersing polyester resin, a dispersing agent, a stabilizing agent and a diluting agent;
step 2: adding the filler and continuously dispersing for 0.5-1 h;
and step 3: vacuumizing for 15-30min to obtain the component A.
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| CN201911073693.6A CN110616005B (en) | 2019-11-06 | 2019-11-06 | High-iron putty and preparation method thereof |
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Citations (5)
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|---|---|---|---|---|
| US3287292A (en) * | 1960-06-27 | 1966-11-22 | Reichhold Chemicals Inc | Process for preparing copolymers and to the resulting product of polyesters containing polymerizable groups and alpha, beta-ethylenically unsaturated compounds |
| CN101704940A (en) * | 2009-11-13 | 2010-05-12 | 常州工程职业技术学院 | Unsaturated polyester resin for atomic ash |
| CN102250504A (en) * | 2011-06-20 | 2011-11-23 | 石家庄市油漆厂 | High temperature resistant automobile special putty not influencing adhesion and preparation method thereof |
| CN107987219A (en) * | 2017-12-29 | 2018-05-04 | 吴迪 | A kind of preparation method of the special unsaturated-resin of automobile Putty |
| CN109535400A (en) * | 2018-11-29 | 2019-03-29 | 三棵树涂料股份有限公司 | A kind of preparation method of unsaturated polyester resin |
-
2019
- 2019-11-06 CN CN201911073693.6A patent/CN110616005B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3287292A (en) * | 1960-06-27 | 1966-11-22 | Reichhold Chemicals Inc | Process for preparing copolymers and to the resulting product of polyesters containing polymerizable groups and alpha, beta-ethylenically unsaturated compounds |
| CN101704940A (en) * | 2009-11-13 | 2010-05-12 | 常州工程职业技术学院 | Unsaturated polyester resin for atomic ash |
| CN102250504A (en) * | 2011-06-20 | 2011-11-23 | 石家庄市油漆厂 | High temperature resistant automobile special putty not influencing adhesion and preparation method thereof |
| CN107987219A (en) * | 2017-12-29 | 2018-05-04 | 吴迪 | A kind of preparation method of the special unsaturated-resin of automobile Putty |
| CN109535400A (en) * | 2018-11-29 | 2019-03-29 | 三棵树涂料股份有限公司 | A kind of preparation method of unsaturated polyester resin |
Non-Patent Citations (1)
| Title |
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| 原燃料化学工业部涂料技术训练班: "《涂料工艺 第五分册》", 30 April 1976, 石油化学工业出版社 * |
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Denomination of invention: A kind of high iron atom ash and its preparation method Effective date of registration: 20220728 Granted publication date: 20210622 Pledgee: Bank of China Limited Qingyuan Branch Pledgor: QINGYUAN YONGCHANG PAINT CO.,LTD. Registration number: Y2022980011440 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A High Iron Atomic Ash and Its Preparation Method Effective date of registration: 20230925 Granted publication date: 20210622 Pledgee: Bank of China Limited Qingyuan Branch Pledgor: QINGYUAN YONGCHANG PAINT CO.,LTD. Registration number: Y2023980058445 |