CN112111065A - Preparation method of polyether modified organic silicon flatting agent - Google Patents
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Abstract
The invention provides a preparation method of a polyether modified organic silicon flatting agent, and belongs to the technical field of flatting agents. The invention comprises the following steps: mixing first double-end hydrogen-containing silicone oil, second double-end hydrogen-containing silicone oil, first side chain hydrogen-containing silicone oil and second side chain hydrogen-containing silicone oil, adding a chloroplatinic acid catalyst, heating to 75-80 ℃, dropwise adding an allyl polyether mixture to perform hydrosilylation reaction for 4-5 hours, wherein the reaction temperature is 80-95 ℃; cooling to room temperature to obtain polyether modified organic silicon; the molecular weights of the first double-end hydrogen-containing silicone oil and the second double-end hydrogen-containing silicone oil are different, and the molecular weights of the first side chain hydrogen-containing silicone oil and the second side chain hydrogen-containing silicone oil are different. The polyether modified organic silicon flatting agent disclosed by the invention has better defoaming and foam inhibiting performances in an aqueous coating system, shows good foam control capability, and also shows excellent cold and heat resistance, and does not crack, adhere or shrink the hole.
Description
Technical Field
The invention belongs to the technical field of leveling agents, and particularly relates to a preparation method of a polyether modified organic silicon leveling agent.
Background
The leveling agent is an auxiliary agent commonly used in the coating. The main functions of the paint are decoration and protection, after the paint is constructed, a new interface can appear, generally speaking, the new interface is a liquid/solid interface between the paint and a substrate and a liquid/air interface between the paint and air, if the flowing and leveling defects occur, the paint film thickness is insufficient, pinholes are formed, the discontinuity of the paint film can be caused, the appearance is influenced, and the protection function is also damaged. Particularly, with the rapid development of water-based paint, various strong polar polymer resins and solvents with high surface tension are widely used, the system is easy to foam, the substrate is difficult to wet, and a leveling agent is added, so that the paint is promoted to flow and dry to form a flat coating film by adjusting the paint properties and changing the paint in the construction and film forming processes, and the paint is helped to obtain good leveling.
Wherein, the modified organosilicon is the most extensive leveling agent with better smooth flowing effect in the coating industry. The surface tension of the coating can be reduced, the surface tension gradient of the coating is reduced, the formation of a Benard spiral pit is prevented, the leveling and luster are improved, the interfacial tension of a coating and a base material is reduced, the wetting to the base material is improved, and the surface morbidity of the coating such as shrinkage cavity is reduced. Paint film defects such as cratering, orange peel, pinholes, fogging, etc. are easily caused by paint flow in the wet paint film during the process of paint flow and drying to form a film after the paint is applied. The leveling agent is added to promote the coating to form a flat, smooth and uniform coating film in the drying film-forming process, so that the defects of the coating film are prevented.
The structure of the common organic silicon flatting agent in the current market is mainly the most common polyether modified silicone oil, for example, the patent with the application number of CN201510891948 discloses an organic silicon flatting agent and a preparation method thereof, polyether poly modified organic siloxane with different end-capping structures is obtained by reacting side chain hydrogen-containing silicone oil and allyl polyether, and the organic silicon flatting agent has good application performance in powder coating and baking varnish. Chinese patent with application number CN201910621718 discloses an organosilicon leveling agent and a coating with good recoatability, and the preparation method adopts a straight chain modification technology, and comprises the steps of preparing the organosilicon leveling agent from hydrogen-containing silicone oil with double ends and allyl polyether under the action of a chloroplatinic acid catalyst, wherein the modified organosilicon has increased hydrophilicity, and can improve the surface energy of the coated coating surface and improve the recoatability of the coating after being added into the coating. The invention discloses a terminal modified organic silicon coating leveling agent and a preparation method thereof in a patent with the application number of CN201210134489.2, and relates to a coating leveling agent, in particular to the preparation of polyether terminal modified polydimethylsiloxane and the application of the polyether terminal modified polydimethylsiloxane as the leveling agent in coating. The leveling agent has the advantages of reducing the surface tension of the coating, improving the wettability of the substrate, improving the flowing and leveling of the coating and removing surface defects; increasing the sliding property, reducing the surface friction coefficient of the coating, and improving the scratch resistance and the adhesion resistance.
In addition, polyester, long chain alkyl, aralkyl, hydroxyl or vinyl and other modified groups are used for modifying the side chain or the straight chain of the silicone oil to obtain the modified organic silicon leveling agent. The leveling property of the modified organic silicon can meet the use requirement by adjusting the type, the number and the modification position of the modification group.
In the prior art, the organic silicon flatting agent cannot participate in the curing process of the resin coating or the printing ink after being added into the coating, has poor compatibility with the resin coating or the printing ink, low density during use, poor strength of a formed film, easy generation of bubbles in the coating, easy falling and peeling after being coated on the surface of an object, poor cold and hot resistance, short service life under the condition of extremely low temperature or extremely high temperature, easy cracking, and easy turbidity of the coating or the printing ink system caused by excessive addition, and influences the appearance of a final product.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a polyether modified organic silicon flatting agent, which is a multifunctional organic silicon flatting agent prepared by polysiloxane main chains and polyether groups.
The invention relates to a preparation method of a polyether modified organic silicon flatting agent, which comprises the following steps:
mixing first double-end hydrogen-containing silicone oil, second double-end hydrogen-containing silicone oil, first side chain hydrogen-containing silicone oil and second side chain hydrogen-containing silicone oil, adding a chloroplatinic acid catalyst, heating to 75-80 ℃, dropwise adding an allyl polyether mixture to perform hydrosilylation reaction for 4-5 hours, wherein the reaction temperature is 80-95 ℃; cooling to room temperature to obtain polyether modified organic silicon;
the molecular weights of the first double-end hydrogen-containing silicone oil and the second double-end hydrogen-containing silicone oil are different, and the molecular weights of the first side chain hydrogen-containing silicone oil and the second side chain hydrogen-containing silicone oil are different.
The molecular weight of the first double-end hydrogen-containing silicone oil is 1000-4000, the molecular weight of the second double-end hydrogen-containing silicone oil is 4000-8000, the molecular weight of the first side chain hydrogen-containing silicone oil is 1000-2500, and the molecular weight of the second side chain hydrogen-containing silicone oil is 2500-5000.
The mass ratio of the first double-end hydrogen-containing silicone oil to the second double-end hydrogen-containing silicone oil to the first side chain hydrogen-containing silicone oil to the second side chain hydrogen-containing silicone oil is 1-2: 1-2: 0.25-0.6: 0.35-0.6.
The mass ratio of the first double-end hydrogen-containing silicone oil to the second double-end hydrogen-containing silicone oil to the first side chain hydrogen-containing silicone oil to the second side chain hydrogen-containing silicone oil is 1: 2: 0.6: 0.6.
the allyl polyether mixture is a mixture of allyl polyethers of different degrees of saturation.
The structural formula of the first double-end hydrogen-containing silicone oil is as follows:
The structural formula of the second double-end hydrogen-containing silicone oil refers to the structural formula.
The structural formula of the first side chain hydrogen-containing silicone oil is as follows:
The structural formula of the second side chain hydrogen-containing silicone oil refers to the structural formula.
Allyl polyethers are specified to have the following structural formula:
Good compatibility and low surface tension are two key indexes for exerting the leveling performance. The migration orientation of the leveling agent follows the "energy minimum principle" in physics, namely, the leveling agent spontaneously flows from a place with high energy to a place with low energy, and only the leveling agent spontaneously migrates to the surface of a paint film, the leveling effect can be generated, so that the paint is promoted to form a flat, smooth and uniform coating film in the drying and film forming process, and the leveling agents suitable for different types of paint are different. In terms of structure-activity relationship, the action effect of the leveling agent is mainly determined by the chemical structure of the modified polysiloxane. For example, the molecular weight of the polysiloxane, the type, size, position and number of the modified organic groups and the linking mode of the organic modified polysiloxane all influence the leveling performance effect of the polysiloxane. The value of q of the chain link of the terminal hydrogen silicone oil, the m/n ratio of the side chain hydrogen silicone oil and the x/y ratio of the chain link of the allyl polyether are all reflected on the molecular structure of the polysiloxane, and the important influences are exerted on the key performances of the polyether modified organic silicon leveling agent, such as compatibility, leveling capability, foam stabilizing capability, recoating performance and the like. For example, the smaller the q value and the m/n value, the better the compatibility, and in the case that the q value and the m/n value are fixed, the larger the x/y value, the better the compatibility, and the larger the x + y value, the better the leveling effect. However, the larger the value of m + n and the higher the value of m/n, the more likely the problem of poor recoatability arises. Under the condition of a fixed x/y value, the q value and the m/n ratio have influence on the foam stabilizing performance. Therefore, the influence of the values or ratios of q, m, n, x and y on each performance index of the leveling agent is complex, the adverse aspects of mutual contradiction and the synergistic and synergistic benefits exist, and how to balance the rationality between the values or ratios can be obtained through comprehensive performance evaluation data on the basis of a large number of tests. The invention prepares various polyether modified organic silicon flatting agents by innovatively and preferably selecting the molecular weight range of two main raw materials of polysiloxane (side chain or straight chain type hydrogen-containing silicone oil) and the key technical index of the unsaturation degree of methyl-terminated allyl polyether, linking the technical indexes of the raw materials with the molecular structure, controlling the overall key index, and giving play to the unique advantages of straight chain and side chain types and synergizing, thereby preferably selecting the optimal application performance scheme.
Has the beneficial effects that; the polyether modified organic silicon flatting agent disclosed by the invention has better defoaming and foam inhibiting performances in an aqueous coating system, shows good foam control capability, also shows excellent cold and heat resistance, and has excellent performances of no cracking, no stickiness and no shrinkage cavity.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
The hydrogen content and the double bond content of the material can be measured according to the following methods when selecting the raw materials:
the method for measuring the hydrogen content comprises the following steps:
accurately weighing about 0.2g (accurate to 0.0002 g) of sample, placing in a 250mL iodine vial, adding 20mL of LCCl4Dissolving, adding 10.00mL of bromo-acetic acid (0.2mol/L), standing at room temperature in the dark for 1 hour, accurately adding 15.00mL of 20% KI solution by using a pipette, washing the bottle mouth with deionized water, and using 0.1mol/LNa2S2O3The standard solution was titrated with starch as indicator and titrated to the end point where the blue color disappeared.
Calculating, the mass percentage of hydrogen is expressed as H percent,
in the formula: C-Na2S2O3Standard solution concentration (mol/L);
V1-volume of blank sodium thiosulfate standard solution consumed (mL);
V2-volume of sample consuming sodium thiosulfate standard solution (mL);
m-sample mass (g).
The double bond content measuring method comprises the following steps:
accurately weighing about 0.5g (accurate to 0.0002 g) of sample, placing in a 250mL iodine vial, adding 20mL of LCCl4Dissolving, adding 15.00mL of bromo-acetic acid (0.2mol/L), standing at room temperature in the dark for 1 hour, accurately adding 15.00mL of 20% KI solution by using a pipette, washing the bottle mouth with deionized water, and using 0.1mol/LNa2S2O3The standard solution was titrated with starch as indicator and titrated to the end point where the blue color disappeared.
And (3) calculating: the double bond content is expressed as X (mmol/g)
In the formula: C-Na2S2O3Standard solution concentration (mol/L);
V1-volume of blank sodium thiosulfate standard solution consumed (mL);
V2-volume of sample consuming sodium thiosulfate standard solution (mL);
m-sample mass (g).
The moisture measurement method comprises the following steps:
the determination is carried out by referring to GB/T11275-2007 ' determination of water content of surfactant ' 7.1 Karl Fischer ' method. The feeding mode is as follows:
the reaction feeding mode of the allyl polyether and the hydrogen-containing silicone oil is mainly three: one-time charging method of allyl polyether and hydrogen-containing silicone oil; a method of dropwise adding hydrogen-containing silicone oil; the method of dropping allyl polyether. Under the action of proper temperature and catalyst, Si-H in the hydrogen-containing silicone oil and C = C in the allyl polyether can be reacted completely basically, and the key point of maintaining the catalytic activity and the feeding speed is the success or failure of the reaction. The feeding mode is that allyl polyether is dripped into a hydrogen-containing silicone oil reaction system.
The first double-end hydrogen-containing silicone oil and the second double-end hydrogen-containing silicone oil have the following structural formulas:
wherein q = 12-52.
The first side chain hydrogen-containing silicone oil and the second side chain hydrogen-containing silicone oil have the following structural formulas:
wherein m =4-20 and n = 4-20.
Allyl polyethers of different unsaturation are specifically designated as having the following structural formula:
wherein x =12-80 and y = 1-20.
Wherein, the values of q, m, n, x and y need to be determined according to specific substance calculation, and the range of the values is suitable for the range of molecular weight.
The allyl polyether refers in particular to the following specific technical indexes
The feeding mode is as follows:
example 1
100G of first double-end hydrogen-containing silicone oil with the molecular weight of 1000, 200G of second double-end hydrogen-containing silicone oil with the molecular weight of 4100, 50G of first side-chain hydrogen-containing silicone oil with the molecular weight of 1000, 40G of second side-chain hydrogen-containing silicone oil with the molecular weight of 2600 and 10ppm of chloroplatinic acid catalyst (the chloroplatinic acid catalyst is calculated according to the mass of the effective components of platinum in the total reaction materials), introducing nitrogen, stirring and heating to 80 ℃, dropwise adding 30G of allyl polyether 1 and 28G of allyl polyether 2 and the chloroplatinic acid catalyst (the chloroplatinic acid catalyst is 10ppm of the mass of the total reaction materials), dropwise adding for 1h, continuously stirring and carrying out heat preservation reaction for 4.5h, controlling the reaction temperature to be 80 ℃, stopping heating, vacuum-pumping low-boiling-point substances, cooling, checking and discharging to prepare 440G of light yellow transparent polyether modified silicone viscous liquid G1.
Wherein the content of the first and second substances,
g1 polyether modified organosilicon quality index
Example 2
100G of 4000G of first double-end hydrogenous silicone oil with molecular weight of 4000, 200G of 8000G of second double-end hydrogenous silicone oil with molecular weight of 8000, 50G of 2500G of first side chain hydrogenous silicone oil with molecular weight of 2500, 35G of 5000G of second side chain hydrogenous silicone oil with molecular weight of 5000 and 10ppm of chloroplatinic acid catalyst (the chloroplatinic acid catalyst is calculated according to the effective component of platinum in the mass of the total reaction materials), introducing nitrogen, stirring and heating to 80 ℃, dropwise adding 20G of allyl polyether 1 and 28G of allyl polyether 3 and the chloroplatinic acid catalyst (the chloroplatinic acid catalyst is 10ppm of the mass of the total reaction materials), dropwise adding for 1h, continuously stirring and carrying out heat preservation reaction for 5h, controlling the reaction temperature to be 95 ℃, stopping heating, vacuum-pumping out low-boiling-point substances, cooling, checking and discharging to obtain 423G of light yellow transparent polyether modified organosilicon viscous liquid G2.
G2 polyether modified organosilicon quality index
Example 3
150G of 3500 molecular weight first double-end hydrogen-containing silicone oil, 150G of 7000 molecular weight second double-end hydrogen-containing silicone oil, 50G of 200 molecular weight first side chain hydrogen-containing silicone oil, 40G of 4000 molecular weight second side chain hydrogen-containing silicone oil and 10ppm chloroplatinic acid catalyst (the chloroplatinic acid catalyst is calculated according to the effective components of platinum in the total mass of reaction materials), introducing nitrogen, stirring and heating to 76 ℃, dropwise adding 25G of allyl polyether 2 and 26G of allyl polyether 3 and chloroplatinic acid catalyst (the chloroplatinic acid catalyst is 10ppm of the total mass of the reaction materials), dropwise adding for 1h, continuously stirring and carrying out heat preservation reaction for 4h, controlling the reaction temperature to 85 ℃, stopping heating, vacuum-pumping out low-boiling-point substances, cooling, checking and discharging to obtain 433G of light yellow transparent polyether modified silicone viscous liquid G3.
G3 polyether modified organosilicon quality index
Example 4
100G of first double-end hydrogen-containing silicone oil with the molecular weight of 3000, 200G of second double-end hydrogen-containing silicone oil with the molecular weight of 7000, 45G of first side chain hydrogen-containing silicone oil with the molecular weight of 2300, 35G of second side chain hydrogen-containing silicone oil with the molecular weight of 4000 and 10ppm of chloroplatinic acid catalyst (the chloroplatinic acid catalyst is calculated according to the mass ratio of the effective components of platinum in the total reaction materials) are added into a 500mL four-neck flask, nitrogen is introduced, the mixture is stirred and heated to 75 ℃, 20G of allyl polyether 1 and 28G of allyl polyether 4 and chloroplatinic acid catalyst (the chloroplatinic acid catalyst is 10ppm of the mass ratio of the total reaction materials) are added dropwise for 1h, the stirring and heat preservation reaction are continued for 5h, the reaction temperature is controlled to be 80 ℃, the heating is stopped, low-boiling-point substances are removed in vacuum, and the temperature is reduced, inspected.
G4 polyether modified organosilicon quality index
Example 5
100G of first double-end hydrogen-containing silicone oil with the molecular weight of 3000, 200G of second double-end hydrogen-containing silicone oil with the molecular weight of 6000, 60G of first side-chain hydrogen-containing silicone oil with the molecular weight of 2000, 60G of second side-chain hydrogen-containing silicone oil with the molecular weight of 4000 and 10ppm of chloroplatinic acid catalyst (the chloroplatinic acid catalyst is calculated according to the mass ratio of the effective components of platinum in the total reaction materials) are added into a 500mL four-neck flask, nitrogen is introduced, the mixture is stirred and heated to 80 ℃, 20G of allyl polyether 3 and 21G of allyl polyether 4 and the chloroplatinic acid catalyst (the chloroplatinic acid catalyst is 10ppm of the mass ratio of the total reaction materials) are dropwise added for 1h, the stirring and heat preservation reaction are continued for 5h, the reaction temperature is controlled to 85 ℃, the heating is stopped, low-boiling-point substances are removed in vacuum, the temperature is reduced, the inspection.
G5 polyether modified organosilicon quality index
Example 6
150G of first double-end hydrogen-containing silicone oil with the molecular weight of 2000, 150G of second double-end hydrogen-containing silicone oil with the molecular weight of 6000, 50G of first side chain hydrogen-containing silicone oil with the molecular weight of 2000, 40G of second side chain hydrogen-containing silicone oil with the molecular weight of 5000 and 10ppm of chloroplatinic acid catalyst (the chloroplatinic acid catalyst is calculated according to the mass ratio of the effective components of platinum in the total reaction materials) are added into a 500mL four-neck flask, nitrogen is introduced, the mixture is stirred and heated to 80 ℃, 25G of allyl polyether 1 and 39G of allyl polyether 2 and chloroplatinic acid catalyst (the chloroplatinic acid catalyst is 10ppm of the mass ratio of the total reaction materials) are dripped, the dripping time is 1h, the stirring and heat preservation reaction are continued for 5h, the reaction temperature is controlled to 85 ℃, the heating is stopped, low boiling point substances are pumped out in vacuum, the temperature is reduced, the inspection.
G6 polyether modified organosilicon quality index
Example 7
100G of 3500G of first double-end hydrogen-containing silicone oil with molecular weight of 3500, 200G of 7500G of second double-end hydrogen-containing silicone oil with molecular weight of 7500, 25G of 1800G of first side-chain hydrogen-containing silicone oil with molecular weight of 5000, 60G of 5000 second side-chain hydrogen-containing silicone oil with molecular weight of 5000 and 10ppm of chloroplatinic acid catalyst (the chloroplatinic acid catalyst is calculated according to the effective component of platinum in the total mass of reaction materials), introducing nitrogen, stirring and heating to 80 ℃, dropwise adding 20G of allyl polyether 3 and 19G of allyl polyether 4 and chloroplatinic acid catalyst (the chloroplatinic acid catalyst is 10ppm of the total mass of the reaction materials), dropwise adding for 1h, continuously stirring and carrying out heat preservation reaction for 5h, controlling the reaction temperature to 95 ℃, stopping heating, vacuum-pumping out low-boiling-point substances, cooling, checking and discharging to prepare 410G of light yellow transparent polyether modified silicone viscous liquid G7.
G7 polyether modified organosilicon quality index
Example 8
200G of 3800 molecular weight first double-end hydrogen-containing silicone oil, 100G of 7000 molecular weight second double-end hydrogen-containing silicone oil, 60G of 2000 molecular weight first side chain hydrogen-containing silicone oil, 40G of 4500 molecular weight second side chain hydrogen-containing silicone oil and 10ppm of chloroplatinic acid catalyst (the chloroplatinic acid catalyst is calculated according to the effective component of platinum in the total mass of reaction materials), introducing nitrogen, stirring and heating to 80 ℃, dropwise adding 20G of allyl polyether 2, 18G of allyl polyether 4 and the chloroplatinic acid catalyst (the chloroplatinic acid catalyst is 10ppm of the total mass of the reaction materials), dropwise adding for 1h, continuously stirring and carrying out heat preservation reaction for 5h, controlling the reaction temperature to be 85 ℃, stopping heating, vacuum-pumping low-boiling-point substances, cooling, checking and discharging to obtain 427G of light yellow transparent polyether modified silicone viscous liquid G8.
G8 polyether modified organosilicon quality index
Testing the application performance of the water-based paint:
compatibility test
0.3 percent of the total mass of the leveling agents G1 to G8 prepared in examples 1 to 8 of the invention are respectively added into the alkyd resin, the polyurethane and the acrylic resin to be uniformly stirred, the leveling agents are hung on a glass plate at 105 ℃ for 1h to observe the transparency of the glass plate, a blank test is carried out in the same way, 1 to 5 represents the shape-compatibility effect, 1 represents the worst solubility, 5 represents the best compatibility, and the results are as follows;
it can be seen that the test samples have better compatibility with alkyd, polyurethane and acrylic resins, and in particular sample G1 and sample G2 have performed best.
Leveling property: selecting a polyester resin to prepare white paint (color/base =30/70), wherein the addition amount of the white paint is 0.3% of the solid resin, preparing a paint spraying plate, and observing the leveling effect after 20min at 140 ℃. G1-5 shows the levelling effect, G1 shows the worst levelling and G5 shows the best levelling.
Gloss: coating film 20 measured by paint gloss meteroThe higher the glossiness, the higher the glossiness value, the higher the reflectivity of the coating film, the higher the glossiness of the coating film.
The value: the distinctness of image (DOI) of the film was measured using an orange peel instrument, with higher DOI values indicating a smoother surface of the film.
Heat resistance: the color change on the surface of the coating film is visually identified, wherein 1-5 represents the yellowing degree, 1 represents no yellowing, and 5 represents severe yellowing.
Recoatability: after the primary coating film is dried, the coating film is coated again, the leveling property of the recoat coating film is visually observed, 1-5 represents the effect of recoat performance, 1 represents the worst recoat performance, and 5 represents the best recoat performance.
Comprehensive performance of organosilicon leveling agent
| Sample (I) | Leveling property | Degree of gloss | DOI | Heat resistance | Recoatability |
| Blank space | - | 83 | 75 | 1 | - |
| G1 | 5 | 92 | 85 | 1 | 5 |
| G2 | 5 | 94 | 89 | 1 | 5 |
| G3 | 5 | 94 | 88 | 1 | 5 |
| G4 | 4 | 90 | 84 | 1 | 4 |
| G5 | 5 | 92 | 88 | 1 | 5 |
| G6 | 4 | 89 | 82 | 1 | 4 |
| G7 | 4 | 87 | 80 | 1 | 4 |
| G8 | 5 | 91 | 87 | 1 | 5 |
| Comparison sample A (side chain type) | 3 | 81 | 81 | 5 | 2 |
| COMPARATIVE SAMPLE B (STRAIGHT-CHAIN TYPE) | 4 | 87 | 85 | 4 | 2 |
It can be seen that the polyether modified silicone leveling agent of the present invention exhibited superior leveling, gloss, DOI values, and heat resistance and overcoatability compared to the no-addition leveling agent, and comparative examples a and B.
Foaming test: selecting polyacrylic resin whitening paint (pigment/base =30/70), weighing 0.3% of each leveling agent by mass in resin solids, weighing 500g of the coating (without the defoaming agent) in a 1000mL beaker, starting a stirrer to stir at the rotating speed of 3000r/min for 15 minutes, and then weighing the coating density by using a coating density cup. Under the same condition, the density of the coating is blank without adding a leveling agent.
Cold-hot cycling test: selecting polyacrylic resin white paint (pigment/base =30/70), wherein the using amount of each leveling agent is 0.3% of the mass of resin solids, weighing 500g of coating (without defoaming agent) in a 1000mL beaker, starting a stirrer to stir at the rotating speed of 3000r/min for 15 minutes, uniformly coating on a polyester plate, drying at 50 ℃ for 30 minutes until complete drying, then freezing at-50 ℃ for 24 hours, taking out to see whether cracking occurs, then putting in a 120 ℃ oven for 4 hours, taking out to see whether the surface is sticky or not and shrinkage cavity occurs, and circularly testing for three cycles.
Foaming and heat resistance of organosilicon leveling agent
After the polyether modified organic silicon flatting agent provided by the embodiment of the invention is added into the coating and dispersed at a high speed, the density of the coating is obviously higher than that of the coating without the organic silicon flatting agent, and compared with two common typical side chain polyether modified or straight chain polyether modified organic silicon flatting agents sold in the market, the polyether modified organic silicon flatting agent provided by the invention has better defoaming and foam inhibiting performances in a water-based coating system, shows good foam control capability, simultaneously also shows excellent cold and heat resistance, and has excellent performances of no cracking, no stickiness and no shrinkage cavity.
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.
Claims (9)
1. A preparation method of a polyether modified organic silicon flatting agent is characterized by comprising the following steps:
mixing first double-end hydrogen-containing silicone oil, second double-end hydrogen-containing silicone oil, first side chain hydrogen-containing silicone oil and second side chain hydrogen-containing silicone oil, adding a chloroplatinic acid catalyst, heating to 75-80 ℃, and dropwise adding an allyl polyether mixture to perform hydrosilylation reaction; cooling to room temperature to obtain polyether modified organic silicon;
the molecular weights of the first double-end hydrogen-containing silicone oil and the second double-end hydrogen-containing silicone oil are different, and the molecular weights of the first side chain hydrogen-containing silicone oil and the second side chain hydrogen-containing silicone oil are different.
2. The method as claimed in claim 1, wherein the molecular weight of the first terminal hydrogen-containing silicone oil is 1000-4000, and the molecular weight of the second terminal hydrogen-containing silicone oil is 4100-8000.
3. The method as claimed in claim 2, wherein the molecular weight of the first side chain hydrogen-containing silicone oil is 2500-.
4. The preparation method of the polyether modified organic silicon leveling agent according to claim 3, wherein the mass ratio of the first double-end hydrogen-containing silicone oil to the second double-end hydrogen-containing silicone oil to the first side chain hydrogen-containing silicone oil to the second side chain hydrogen-containing silicone oil is 1-2: 0.25-0.6: 0.35-0.6.
5. The preparation method of the polyether modified organic silicon leveling agent according to claim 4, wherein the mass ratio of the first double-end hydrogen-containing silicone oil to the second double-end hydrogen-containing silicone oil to the first side chain hydrogen-containing silicone oil to the second side chain hydrogen-containing silicone oil is 1: 2: 0.6: 0.6.
6. the method as claimed in claim 5, wherein the allyl polyether mixture is a mixture of allyl polyethers having different degrees of saturation.
7. The preparation method of the polyether modified organic silicon leveling agent according to claim 1, wherein the structural formula of the first double-end hydrogen-containing silicone oil is as follows:
8. the method of claim 1, wherein the polyether modified silicone leveling agent is prepared by the following steps,
the structural formula of the first side chain hydrogen-containing silicone oil is as follows:
9. the method for preparing a polyether modified organic silicon leveling agent according to claim 1, wherein the hydrosilylation reaction time is 4-5 hours, and the reaction temperature is 80-95 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010809531.0A CN112111065A (en) | 2020-08-13 | 2020-08-13 | Preparation method of polyether modified organic silicon flatting agent |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643565A (en) * | 2012-05-04 | 2012-08-22 | 浙江润禾有机硅新材料有限公司 | Terminal modified organic silicone coating flatting agent and preparation method thereof |
| CN105315757A (en) * | 2015-12-06 | 2016-02-10 | 广州市斯洛柯高分子聚合物有限公司 | Organic silicon leveling agent and preparation method thereof |
| CN110256892A (en) * | 2019-07-10 | 2019-09-20 | 广东省科学院产业技术育成中心 | A kind of organosilicon levelling agent and its good coating of overcoating performance |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643565A (en) * | 2012-05-04 | 2012-08-22 | 浙江润禾有机硅新材料有限公司 | Terminal modified organic silicone coating flatting agent and preparation method thereof |
| CN105315757A (en) * | 2015-12-06 | 2016-02-10 | 广州市斯洛柯高分子聚合物有限公司 | Organic silicon leveling agent and preparation method thereof |
| CN110256892A (en) * | 2019-07-10 | 2019-09-20 | 广东省科学院产业技术育成中心 | A kind of organosilicon levelling agent and its good coating of overcoating performance |
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Application publication date: 20201222 |