Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the high-solid-content acrylic pressure-sensitive adhesive and the preparation method thereof, the operation is safe, the product cost is low, the solid content of the prepared acrylic pressure-sensitive adhesive is improved to more than 60 percent, and the drying speed is high.
The technical scheme of the invention is realized as follows:
the high-solid-content acrylic pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 180-200 parts of isooctyl acrylate, 110-130 parts of n-butyl acrylate, 90-120 parts of 2-ethylhexyl acrylate, 80-110 parts of methyl acrylate, 90-110 parts of methyl methacrylate, 60-90 parts of acrylamide, 65-75 parts of acrylic acid, 6-8 parts of sodium dodecyl benzene sulfonate, 8-12 parts of 2-acrylamido-2-methylpropanesulfonic acid, 3-5 parts of cumene hydroperoxide, 4-8 parts of potassium persulfate, 12-16 parts of sodium bicarbonate and 3-6 parts of dodecyl mercaptan.
Preferably, the feed is prepared from the following raw materials in parts by weight: 190 parts of isooctyl acrylate, 120 parts of n-butyl acrylate, 100 parts of 2-ethylhexyl acrylate, 90 parts of methyl acrylate, 100 parts of methyl methacrylate, 75 parts of acrylamide, 70 parts of acrylic acid, 7 parts of sodium dodecyl benzene sulfonate, 10 parts of 2-acrylamido-2-methylpropanesulfonic acid, 4 parts of cumene hydroperoxide, 6 parts of potassium persulfate, 14 parts of sodium bicarbonate and 4 parts of dodecyl mercaptan.
A preparation method of high solid content acrylic pressure-sensitive adhesive comprises the following steps:
(1) weighing isooctyl acrylate, n-butyl acrylate, 2-ethylhexyl acrylate, methyl methacrylate, acrylamide and acrylic acid, sequentially putting into a reactor, and stirring at the speed of 100-120r/min for 10-20min to obtain a mixed monomer;
(2) adding sodium dodecyl benzene sulfonate, 2-acrylamido-2-methylpropanesulfonic acid and distilled water into a reactor, heating to 45-55 ℃, reacting for 20-30min, uniformly mixing the mixed monomers in the step (1), then dripping into the reactor within 50-60min, continuously stirring, controlling the stirring speed at 650-700r/min, and preserving heat for 20-30min after finishing dripping to obtain a pre-emulsion;
(3) adding sodium bicarbonate, dodecyl mercaptan and deionized water into a reaction kettle, heating to 80-85 ℃, controlling the stirring speed to be 250-300 r/min, dropwise adding part of pre-emulsion into the reaction kettle at a certain speed, controlling the speed to be 0.5-1h, slowly dropwise adding cumene hydroperoxide at the same time, controlling the time to be 1-1.5h, carrying out seed emulsion polymerization, and preserving the temperature for 0.5-1h when blue fluorescence appears in the emulsion;
(4) and (3) dripping the residual pre-emulsion and potassium persulfate into the reaction kettle, preserving the heat for 1-2h after dripping within 3-4h, cooling to 50-60 ℃, adjusting the pH value of the product to be neutral by using 25% ammonia water by mass fraction, filtering and discharging to obtain a finished product.
Preferably, the stirring speed in the step (1) is 110r/min, and the stirring time is 15 min.
Preferably, the temperature in the step (2) is increased to 50 ℃ for reaction for 25 min.
Preferably, in the step (3), sodium bicarbonate, dodecyl mercaptan and deionized water are added into a reaction kettle, the temperature is raised to 82 ℃, and the stirring speed is controlled at 280 r/min.
Preferably, 1/10 of the pre-emulsion taken in the step (3) is dropped into the reaction kettle at a certain speed.
Preferably, 1/10 of the pre-emulsion taken in the step (3) is dripped into the reaction kettle within 40 min.
Preferably, cumene hydroperoxide is slowly added dropwise in the step (3) at the same time, and the time is controlled to be 80 min.
Preferably, in the step (4), the residual pre-emulsion and potassium persulfate are dripped into the reaction kettle, the temperature is kept for 1h after dripping within 3h, and the temperature is reduced to 55 ℃.
The invention has the following beneficial effects: the high-solid content acrylic pressure-sensitive adhesive and the preparation method thereof adopt the control of the reaction speed and temperature of emulsification to reduce the condensation phenomenon, and adopt the emulsifier sodium dodecyl benzene sulfonate, the 2-acrylamido-2-methylpropanesulfonic acid, the initiator cumene hydroperoxide and the initiator potassium persulfate in a matching way, so that the solid content of the prepared high-solid content acrylic pressure-sensitive adhesive is improved to more than 60 percent, the drying speed is high, the product cost is low, the operation is safe, and the high-solid content acrylic pressure-sensitive adhesive meets the requirement of high-speed coating.
Detailed Description
For a more clear understanding of the technical features, objects and advantages of the present invention, reference is now made to the following detailed description of the embodiments of the present invention taken in conjunction with the accompanying drawings, which are included to illustrate and not to limit the scope of the present invention.
Example 1
The high-solid-content acrylic pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 180 parts of isooctyl acrylate, 130 parts of n-butyl acrylate, 90 parts of acrylic acid-2-ethylhexyl ester, 110 parts of methyl acrylate, 90 parts of methyl methacrylate, 90 parts of acrylamide, 65 parts of acrylic acid, 8 parts of sodium dodecyl benzene sulfonate, 8 parts of 2-acrylamido-2-methylpropanesulfonic acid, 5 parts of cumene hydroperoxide, 4 parts of potassium persulfate, 16 parts of sodium bicarbonate and 3 parts of dodecyl mercaptan.
A preparation method of high solid content acrylic pressure-sensitive adhesive comprises the following steps:
(1) weighing isooctyl acrylate, n-butyl acrylate, 2-ethylhexyl acrylate, methyl methacrylate, acrylamide and acrylic acid, sequentially placing into a reactor, stirring at a speed of 100r/min for 10min to obtain a mixed monomer
(2) Adding sodium dodecyl benzene sulfonate, 2-acrylamido-2-methylpropanesulfonic acid and a proper amount of distilled water into a reactor, heating to 45 ℃, reacting for 20min, uniformly mixing the mixed monomers in the step (1), then dripping into the reactor within 50min, continuously stirring, controlling the stirring speed at 650r/min, and keeping the temperature for 20min after finishing dripping to obtain a pre-emulsion;
(3) adding sodium bicarbonate, dodecyl mercaptan and deionized water into a reaction kettle, heating to 80 ℃, and controlling the stirring speed at 250 r/min. Dripping 1/10 of pre-emulsion into a reaction kettle at a certain speed for 0.5h, slowly dripping cumene hydroperoxide for 1h, polymerizing seed emulsion, and preserving heat for 0.5h when blue fluorescence appears in the emulsion;
(4) and (3) dripping the residual pre-emulsion and potassium persulfate into the reaction kettle, preserving the heat for 1h within 3h, cooling to 50 ℃, adjusting the pH value of the product to be neutral by using 25 mass percent ammonia water, filtering and discharging to obtain a finished product.
Example 2
The high-solid-content acrylic pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 200 parts of isooctyl acrylate, 110 parts of n-butyl acrylate, 120 parts of 2-ethylhexyl acrylate, 80 parts of methyl acrylate, 110 parts of methyl methacrylate, 60 parts of acrylamide, 75 parts of acrylic acid, 6 parts of sodium dodecyl benzene sulfonate, 12 parts of 2-acrylamido-2-methylpropanesulfonic acid, 3 parts of cumene hydroperoxide, 8 parts of potassium persulfate, 12 parts of sodium bicarbonate and 6 parts of dodecyl mercaptan.
A preparation method of high solid content acrylic pressure-sensitive adhesive comprises the following steps:
(1) weighing isooctyl acrylate, n-butyl acrylate, 2-ethylhexyl acrylate, methyl methacrylate, acrylamide and acrylic acid, sequentially placing into a reactor, stirring at a speed of 120r/min for 20min to obtain a mixed monomer
(2) Adding sodium dodecyl benzene sulfonate, 2-acrylamido-2-methylpropanesulfonic acid and a proper amount of distilled water into a reactor, heating to 55 ℃, reacting for 30min, uniformly mixing the mixed monomers in the step (1), then dripping into the reactor within 50-60min, continuously stirring, controlling the stirring speed at 700r/min, and preserving heat for 30min after finishing dripping to obtain a pre-emulsion;
(3) adding sodium bicarbonate, dodecyl mercaptan and deionized water into a reaction kettle, heating to 85 ℃, and controlling the stirring speed at 300 r/min. Dripping 1/10 of pre-emulsion into a reaction kettle at a certain speed for 1 hour, slowly dripping cumene hydroperoxide for 1.5 hours, polymerizing seed emulsion, and preserving heat for 1 hour when blue fluorescence appears in the emulsion;
(4) and (3) dripping the residual pre-emulsion and potassium persulfate into the reaction kettle, preserving the heat for 2h after dripping within 4h, cooling to 60 ℃, adjusting the pH value of the product to be neutral by using 25 mass percent ammonia water, filtering and discharging to obtain a finished product.
Example 3
The high-solid-content acrylic pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 190 parts of isooctyl acrylate, 120 parts of n-butyl acrylate, 100 parts of 2-ethylhexyl acrylate, 90 parts of methyl acrylate, 100 parts of methyl methacrylate, 75 parts of acrylamide, 70 parts of acrylic acid, 7 parts of sodium dodecyl benzene sulfonate, 10 parts of 2-acrylamido-2-methylpropanesulfonic acid, 4 parts of cumene hydroperoxide, 6 parts of potassium persulfate, 14 parts of sodium bicarbonate and 4 parts of dodecyl mercaptan.
A preparation method of high solid content acrylic pressure-sensitive adhesive comprises the following steps:
(1) weighing isooctyl acrylate, n-butyl acrylate, 2-ethylhexyl acrylate, methyl methacrylate, acrylamide and acrylic acid, sequentially placing into a reactor, stirring at 100-120r/min for 15min to obtain a mixed monomer
(2) Adding sodium dodecyl benzene sulfonate, 2-acrylamido-2-methylpropanesulfonic acid and a proper amount of distilled water into a reactor, heating to 50 ℃, reacting for 20-30min, uniformly mixing the mixed monomers in the step (1), then dripping into the reactor within 55min, continuously stirring, controlling the stirring speed at 680r/min, and preserving heat for 25min after finishing dripping to obtain a pre-emulsion;
(3) adding sodium bicarbonate, dodecyl mercaptan and deionized water into a reaction kettle, heating to 82 ℃, and controlling the stirring speed at 280 r/min. Dripping 1/10 of pre-emulsion into a reaction kettle at a certain speed for 0.8h, slowly dripping cumene hydroperoxide for 1.2h, polymerizing the seed emulsion, and preserving the temperature for 0.7h when the emulsion generates blue fluorescence;
(4) and (3) dripping the residual pre-emulsion and potassium persulfate into the reaction kettle, preserving the heat for 1.5h after dripping within 3.5h, cooling to 55 ℃, adjusting the pH value of the product to be neutral by using 25 mass percent ammonia water, filtering and discharging to obtain a finished product.
First, performance test
The solid content of the high-solid-content-resistant acrylic pressure-sensitive adhesive is measured according to GB/T2793-1995 standard; viscosity measurements were carried out at 25 ℃ using a rotational viscometer model NDJ-1 (Shanghai balance Instrument plant) according to the GB/T2794-1995 Standard. The results are shown in Table 1.
TABLE 1
Item
|
Example 1
|
Example 2
|
Example 3
|
Viscosity (mPa. s)
|
360
|
350
|
355
|
Solid content (%)
|
67
|
65
|
66 |
As can be seen from Table 1, the high-solid-content acrylic pressure-sensitive adhesive prepared in the embodiments 1 to 3 of the present invention has a good solid content of not less than 65% and a viscosity of less than 400mPa · s, and is suitable for the requirement of high-speed coating.
The above embodiments are merely provided to help understand the method and core principle of the present invention, and the main steps and embodiments of the present invention are described in detail by using specific examples. To those skilled in the art, the various conditions and parameters may be varied as desired in a particular implementation in accordance with the principles of the invention, and in view of the foregoing, the description is not to be taken as limiting the invention.