阅读说明：本技术 一种新型低温易打磨净味醇酸树脂和制备方法 (Novel low-temperature easily-polished odor-removing alkyd resin and preparation method thereof ) 是由 方学平 李玉辉 于 2020-07-03 设计创作，主要内容包括：本发明提供了一种新型低温易打磨净味醇酸树脂,所述醇酸树脂由下列重量份的原料组成：6-10重量份的C8脂肪酸,11-18重量份的净味植物油脂,4-10重量份含多羟基醚,8-12重量份的扩链剂,25-35重量份的分子内酸酐,10-15重量份的季戊四醇,0.01-0.05重量份的减色剂,22-33重量份的溶剂。本发明采用C8饱和脂肪酸,解决传统醇酸树脂因反应不彻底易析出现象,降低异味,同时配合多羟基醚、扩链剂、季戊四醇,提高醇酸树脂的稳定性。(The invention provides a novel low-temperature easy-polishing odor-removing alkyd resin, which is prepared from the following raw materials in parts by weight: 6-10 parts of C8 fatty acid, 11-18 parts of odorless vegetable oil, 4-10 parts of polyhydroxy ether, 8-12 parts of chain extender, 25-35 parts of intramolecular anhydride, 10-15 parts of pentaerythritol, 0.01-0.05 part of color reducing agent and 22-33 parts of solvent. The preparation method adopts C8 saturated fatty acid, solves the problem that the traditional alkyd resin is not completely easy to separate out due to incomplete reaction, reduces peculiar smell, and improves the stability of the alkyd resin by matching with polyhydroxy ether, a chain extender and pentaerythritol.)

1. The novel low-temperature flavor-clearing alkyd resin easy to polish is characterized by comprising the following raw materials in parts by weight: 6-10 parts of C8 fatty acid, 11-18 parts of odorless vegetable oil, 4-10 parts of polyhydroxy ether, 8-12 parts of chain extender, 25-35 parts of intramolecular anhydride, 10-15 parts of pentaerythritol, 0.01-0.05 part of color reducing agent and 22-33 parts of solvent.

2. The alkyd resin of claim 1, wherein said polyhydroxy ether is diethylene glycol and said C8 fatty acid is isooctanoic acid.

3. The alkyd resin of claim 1, wherein said chain extender is trimethylolpropane.

4. The alkyd resin of claim 1, wherein said intramolecular anhydride is phthalic anhydride.

5. The alkyd resin of claim 1, wherein said color-reducing agent is hypophosphorous acid.

6. The alkyd resin of claim 1, wherein said solvent is xylene.

7. A process for the preparation of an alkyd resin according to any of claims 1 to 6, comprising the steps of:

step 1: adding C8 fatty acid, odorless vegetable oil, polyhydroxy ether, a chain extender, intramolecular anhydride, pentaerythritol and 2-3 parts by weight of solvent into a reaction kettle and mixing;

step 2: adding hypophosphorous acid into the system obtained in the step 1, and ensuring that the temperature of the system does not exceed 50 ℃ in the adding process;

and step 3: slowly heating to 130 ℃ at the speed of 10 ℃ per hour, starting stirring, uniformly heating to 160 ℃, starting refluxing, continuously and slowly heating to the kettle temperature of 190-200 ℃, keeping the temperature for 2 hours, carrying out esterification reaction, and removing water generated by the reaction;

and 4, step 4: raising the temperature of the reaction kettle to 210 ℃, preserving the heat for 2 hours, and extracting a sample from the reaction kettle through a vacuum sampling system until the reaction is complete;

and 5: and cooling the system to below 160 ℃, adding the rest dimethylbenzene, and uniformly stirring to obtain the novel low-temperature flavor-clearing alkyd resin easy to polish.

8. The method of claim 7, wherein the steps are as follows:

step 1: introducing carbon dioxide into a reaction kettle at a flow rate of 5L/min for 15 minutes, adding C8 fatty acid, odorless vegetable oil, polyhydroxy ether, a chain extender, intramolecular anhydride, pentaerythritol and 1-3 parts by weight of solvent into the reaction kettle, and mixing;

step 2: adding hypophosphorous acid into the system obtained in the step 1, and ensuring that the temperature of the system does not exceed 50 ℃ in the adding process;

and step 3: slowly heating to 130 ℃ at the speed of 10 ℃ per hour, starting stirring, uniformly heating to 160 ℃, closing carbon dioxide, starting refluxing, continuously and slowly heating to the kettle temperature of 190-200 ℃, keeping the temperature for 2 hours to perform esterification reaction, and removing water generated by the reaction;

and 4, step 4: raising the temperature of the reaction kettle to 210 ℃, preserving the temperature for 2 hours, and extracting a sample from the reaction kettle to perform intermediate detection until the reaction is complete;

and 5: and cooling the system to below 160 ℃, adding the rest dimethylbenzene, and uniformly stirring to obtain the novel low-temperature flavor-clearing alkyd resin easy to polish.

9. The method of claim 7, wherein the step 4 intermediate detection and step 5 are as follows:

sampling and detecting from the reaction kettle once every hour in the esterification process, measuring the acid value and viscosity of the system, and detecting once every 0.5 hour when the viscosity of the Grignard tube reaches 25 s; and when the intermediate control process samples and tests that the Grignard viscosity reaches 35-40s and the acid value is less than 12mgKOH/g, starting a cooling system for cooling, introducing carbon dioxide gas at 5L/min, stopping introducing the carbon dioxide gas when the temperature of the reaction kettle is reduced to 160 ℃, transferring the system from the reaction kettle to a diluting kettle, putting the residual dimethylbenzene into the diluting kettle, starting the diluting kettle and stirring to obtain the novel low-temperature easily-polished pure alkyd resin.

10. The transparent seal primer is characterized by comprising the following raw materials in parts by weight: 50-60 parts by weight of alkyd resin as claimed in any one of claims 1-6, 10-20 parts by weight of castor oil resin, 2-3 parts by weight of anti-settling slurry, 0.1-0.3 part by weight of dispersant, 0.5-1 part by weight of defoaming agent, 10-15 parts by weight of filler, 5-10 parts by weight of zinc stearate, 0.5-1 part by weight of drier and 12-13 parts by weight of BAC.

Technical Field

The invention relates to alkyd resin, in particular to novel low-temperature alcohol acid resin easy to polish and clean in flavor and a preparation method thereof, and belongs to the field of furniture decoration and wood coating.

Background

In the field of furniture decoration and woodware coating, the workability of the paint is good or bad, and whether the performance of the selected resin is sufficient or not is determined, the main performance of the woodware coating is reflected by selecting a resin for application, and the application performance of the resin is improved, namely the market share of the corresponding coating is improved. The prior woodware coating market has the defect that the abrasive paper is difficult to be polished in the aspects of low-temperature construction spraying primer in winter, thin spraying, thick coating and the like. According to market demand analysis, the paint is developed by combining with an environment-friendly type and is applied to the technical field of wood coating manufacturing industry.

The alkyd resin is transparent resin formed by polycondensing polyalcohol, polybasic acid and monobasic acid, and the problems of polishing difficulty and peculiar smell remained after board spraying in the conventional alkyd resin are caused by incomplete reaction.

Disclosure of Invention

The invention provides a novel low-temperature easily-polished odor-removing alkyd resin and a preparation method thereof, which at least solve the problems of polishing difficulty and residual odor after plate spraying.

The invention provides a novel low-temperature easy-polishing odor-removing alkyd resin, which is prepared from the following raw materials in parts by weight: 6-10 parts of C8 fatty acid, 11-18 parts of odorless vegetable oil, 4-10 parts of polyhydroxy ether, 8-12 parts of chain extender, 25-35 parts of intramolecular anhydride, 10-15 parts of pentaerythritol, 0.01-0.05 part of color reducing agent and 22-33 parts of solvent.

Further, the polyhydroxy-containing ether is diethylene glycol, and the C8 fatty acid is isooctanoic acid.

Further, the chain extender is trimethylolpropane.

Further, the intramolecular anhydride is phthalic anhydride.

Further, the color reducing agent is hypophosphorous acid.

Further, the solvent is xylene.

The invention also discloses a preparation method of the alkyd resin, which comprises the following steps:

step 1: adding C8 fatty acid, odorless vegetable oil, polyhydroxy ether, a chain extender, intramolecular anhydride, pentaerythritol and 2-3 parts by weight of solvent into a reaction kettle and mixing;

step 2: adding hypophosphorous acid into the system obtained in the step 1, and ensuring that the temperature of the system does not exceed 50 ℃ in the adding process;

and step 3: slowly heating to 130 ℃ at the speed of 10 ℃ per hour, starting stirring, uniformly heating to 160 ℃, starting refluxing, continuously and slowly heating to the kettle temperature of 190-200 ℃, keeping the temperature for 2 hours, carrying out esterification reaction, and removing water generated by the reaction;

and 4, step 4: raising the temperature of the reaction kettle to 210 ℃, preserving the heat for 2 hours, and extracting a sample from the reaction kettle through a vacuum sampling system until the reaction is complete;

and 5: and cooling the system to below 160 ℃, adding the rest dimethylbenzene, and uniformly stirring to obtain the novel low-temperature flavor-clearing alkyd resin easy to polish.

Further, the steps are as follows:

step 1: introducing carbon dioxide into a reaction kettle at a flow rate of 5L/min for 15 minutes, adding C8 fatty acid, odorless vegetable oil, polyhydroxy ether, a chain extender, intramolecular anhydride, pentaerythritol and 1-3 parts by weight of solvent into the reaction kettle, and mixing;

step 2: adding hypophosphorous acid into the system obtained in the step 1, and ensuring that the temperature of the system does not exceed 50 ℃ in the adding process;

and step 3: slowly heating to 130 ℃ at the speed of 10 ℃ per hour, starting stirring, uniformly heating to 160 ℃, closing carbon dioxide, starting refluxing, continuously and slowly heating to the kettle temperature of 190-200 ℃, keeping the temperature for 2 hours to perform esterification reaction, and removing water generated by the reaction;

and 4, step 4: raising the temperature of the reaction kettle to 210 ℃, preserving the temperature for 2 hours, and extracting a sample from the reaction kettle to perform intermediate detection until the reaction is complete;

and 5: and cooling the system to below 160 ℃, adding the rest dimethylbenzene, and uniformly stirring to obtain the novel low-temperature flavor-clearing alkyd resin easy to polish.

Further, the intermediate detection in step 4 and step 5 are as follows:

sampling and detecting from the reaction kettle once every hour in the esterification process, measuring the acid value and viscosity of the system, and detecting once every 0.5 hour when the viscosity of the Grignard tube reaches 25 s; and when the intermediate control process samples and tests that the Grignard viscosity reaches 35-40s and the acid value is less than 12mgKOH/g, starting a cooling system for cooling, introducing carbon dioxide gas at 5L/min, stopping introducing the carbon dioxide gas when the temperature of the reaction kettle is reduced to 160 ℃, transferring the system from the reaction kettle to a diluting kettle, putting the residual dimethylbenzene into the diluting kettle, starting the diluting kettle and stirring to obtain the novel low-temperature easily-polished pure alkyd resin.

The invention also discloses a closed transparent primer which is prepared from the following raw materials in parts by weight: 50-60 parts by weight of alkyd resin as claimed in any one of claims 1-6, 10-20 parts by weight of castor oil resin, 2-3 parts by weight of anti-settling slurry, 0.1-0.3 part by weight of dispersant, 0.5-1 part by weight of defoaming agent, 10-15 parts by weight of filler, 5-10 parts by weight of zinc stearate, 0.5-1 part by weight of drier and 12-13 parts by weight of BAC.

Compared with the prior art, the alkyd resin adopts C8 saturated fatty acid, solves the problem that the traditional alkyd resin is not completely easy to separate out due to incomplete reaction, reduces peculiar smell, and improves the stability of the alkyd resin by matching with polyhydroxy ether, a chain extender and pentaerythritol.

Detailed Description

In order to make the technical solutions of the present invention better understood by those skilled in the art, 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.

The preparation method of the alkyd resin provided by the embodiment of the invention comprises the following steps:

in the production process, firstly, carbon dioxide is checked and introduced for 15 minutes (flow rate is 5L/min), then vegetable oil, isooctanoic acid, diethylene glycol, phthalic anhydride, pentaerythritol, trimethylolpropane and xylene are accurately added into a reaction kettle, and hypophosphorous acid is added into the reaction kettle at the temperature of less than 50 ℃. After the materials are accurately put into the reaction kettle, the emptying valves of the reaction kettle are checked to be kept in an open state (because the production of the product is carried out under normal pressure), each unloading valve is kept closed, a heating system is checked to be normal, and the water flow of a circulating water system is ensured to be normal. Opening a vertical condenser and a horizontal condenser by using a cooling water valve, opening a heating system to slowly raise the temperature to 130 ℃ at the speed of 10 ℃ per hour, starting stirring, uniformly raising the temperature to 160 ℃, starting backflow and closing carbon dioxide, continuously and slowly raising the temperature to 190-200 ℃ and keeping the temperature for 2 hours to carry out esterification reaction, collecting gas (water and dimethylbenzene) evaporated in the esterification stage in an automatic separator through cooling of the vertical condenser and the horizontal condenser (gas cooling is converted into liquid), separating the esterification water and the dimethylbenzene in the automatic separator (the water density is higher than that of the dimethylbenzene and the two are not dissolved), carrying out structural isolation through the automatic separator, automatically discharging the esterification water into an esterification water collecting storage tank, overflowing the dimethylbenzene to the reaction kettle to continuously evaporate water generated in the kettle in an azeotropic manner, and helping esterification dehydration and circulation. After the temperature of the reaction kettle is kept between 190 ℃ and 200 ℃ for 2h, slowly raising the temperature of the reaction kettle to 210 ℃ and keeping the temperature for 2h, and extracting a sample from the reaction kettle through a vacuum sampling system for intermediate detection. The intermediate detection is determined by the recipe design and is executed strictly according to the intermediate control method index of the recipe design.

The intermediate control indexes are as follows:

according to the indexes, samples are taken from the reaction kettle at intervals of one hour and are detected, and the samples are detected every 0.5 hour when the viscosity of the Grignard tube reaches 25 s. Sampling is carried out periodically in the esterification process to measure the acid value and the viscosity, after the Grignard viscosity reaches 35-40S and is qualified (the viscosity is higher than 35S and lower than 40S) in the middle control process, a cooling system is started to cool, carbon dioxide gas is introduced (the flow is 5L/min), when the temperature of the reaction kettle is reduced to 160 ℃, the introduction of the carbon dioxide gas is stopped, the reaction kettle is half-transferred into a diluting kettle, diluted dimethylbenzene is put into the diluting kettle, the diluting kettle is started to stir, and the stirring is carried out uniformly to adjust various indexes such as solid content, viscosity and the like to meet the technical standard of finished products designed by a formula.

The technical detection project standards of the finished product of the formula design are as follows:

the embodiment of the invention can avoid a certain oxidative polymerization side reaction by introducing a certain amount of carbon dioxide gas, and can play a role in auxiliary stirring to promote the reaction to be smoothly carried out. Therefore, before feeding, carbon dioxide is introduced to 160 ℃, and the reflux is stabilized and then closed. Because the carbon dioxide has higher density, the carbon dioxide has long retention time on the liquid surface and good isolation effect, and the odor purification and the safety of the product are ensured.

The component ratios of examples 1-5 of the present invention are shown in the following table.

Using the materials	Example 1	Example 2	Example 3	Example 4	Example 5
						Odorless vegetable oil	12.22	12.20	11.22	11.22	12.82
C8	6.66	6.68	7.66	7.66	6.06
						Diethylene glycol	4.29	4.28	4.29	4.29	4.29
Phthalic anhydride	25.34	25.25	25.34	26.34	26.34
						Pentaerythritol	12.65	12.62	11.65	11.65	11.65
Trimethylolpropane	8.60	8.63	9.60	9.60	8.60
						Hypophosphorous acid	0.01	0.01	0.01	0.01	0.01
Xylene(refluxing)	1.93	1.93	1.96	1.90	1.91
						Xylene (Dilute)	28.30	28.30	28.00	28.60	28.32