CN112662345A - Preparation method and application of organic silicon modified acrylate bedplate glue - Google Patents
Preparation method and application of organic silicon modified acrylate bedplate glue Download PDFInfo
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Abstract
The invention discloses a preparation method of organic silicon modified acrylate bedplate glue. The bedplate glue is prepared from 200-380 parts of ionized water, 4-5 parts of an anionic emulsifier, 120-160 parts of butyl acrylate, 80-120 parts of isooctyl acrylate, 20-30 parts of methyl methacrylate, 10-20 parts of styrene, 2-5 parts of acrylic acid, 2-5 parts of an acetoacetylated modified acrylic acid self-crosslinking monomer, 2-4 parts of vinyl triisopropoxysilane, 0.05-0.1 part of potassium persulfate, 0.4-0.6 part of sodium bicarbonate, 0.5-1 part of a cohesion promoter SA 5000.5, 0.1-0.2 part of a preservative MV, 0.1-0.2 part of a water-based defoamer, ammonia water for adjusting pH to 7-8, and 0.5-1 part of an associative thickener according to the weight ratio, and can be applied to high-temperature and high-humidity resistant environments such as a flat net machine, an elliptical machine, an octopus machine and the like in machine printing. The product of the invention has better moisture resistance, thermal stability, higher yellow and high temperature resistance, and the emulsion has higher strength and heat resistance, and has the capability of high viscosity but no anti-viscosity.
Description
Technical Field
The invention relates to the field of adhesives, and particularly relates to a preparation method and application of an organic silicon modified acrylate platen adhesive.
Background
In textile printing, in order to ensure that a fabric is smoothly and firmly attached to a printing table plate, a layer of pressure-sensitive adhesive is coated on the table plate, the pressure-sensitive adhesive can be repeatedly adhered and fixed on the textile for use after being coated on the table plate, and the textile is not polluted, and the pressure-sensitive adhesive is also called as table plate adhesive.
The synthetic polymer platen glue has higher bonding strength and excellent reusability, and particularly the emulsion type acrylate platen glue has good water solubility, no toxicity, material pollution, good bonding force and good repeatability, so the synthetic polymer platen glue is gradually accepted by the printing industry.
In recent years, machine printing equipment is widely applied in the printing industry, and flat screen machines, elliptical machines and octopus machines are available everywhere. The above machine printing equipment needs to use the platen glue during the use process. Because the traditional handprint table glue is not resistant to high temperature, the produced printed products can be adhered to a printing table reversely, the quality of the printed products is seriously influenced, meanwhile, in the printing industry of printing equipment, because the general temperature of printing is 30-40 ℃, in order to prevent printing paste from drying and forming films in the repeated printing process for many times and influencing the printing effect, active humidification is generally adopted, the humidity of a production workshop is kept in a high-humidity environment, and the common water-based table glue is easily whitened and adhered back in the high-humidity environment.
Meanwhile, the prior art mainly has the following problems while solving the problems: 1) in the preparation process, the viscosity of the emulsion is increased by adding emulsified terpene phenol, however, terpene phenol is added into the emulsion by a physical method, and is very easy to precipitate, so that the stability of the product is influenced, and the water resistance of the emulsion is that the phenomenon of generating gel particles by self-crosslinking after being placed for a long time at normal temperature is caused by adding the adhesion promoter 910. 2) Volatile matters such as ethanol, propylene glycol monomethyl ether or isopropanol and the like are added in the preparation process, and the crosslinking monomer is N-hydroxymethyl acrylamide, so that formaldehyde is slowly released during film forming and crosslinking, and the environment is polluted; meanwhile, the water-based acrylate has poor water resistance, and can turn white and reduce the viscosity after being washed by water. 3) In the preparation process, a large amount of isooctyl acrylate is used to effectively reduce the glass transition temperature, but the cost is higher, in addition, vinyl acetate is used as a hard monomer, and the process of removing residual monomers is not carried out after the reaction, so that the table glue has more residual monomers and larger taste.
Disclosure of Invention
Therefore, the invention provides a preparation method and application of an organic silicon modified acrylate platen glue, and aims to solve the problems of poor stability, poor viscosity and pollution of the platen glue in the prior art.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a preparation method of organic silicon modified acrylate platen glue, which comprises the following steps of:
step one, preparation of pre-emulsion A
Adding 100-120 parts of deionized water, 4-5 parts of an anionic emulsifier, 120-160 parts of butyl acrylate, 80-120 parts of isooctyl acrylate, 20-30 parts of methyl methacrylate, 10-20 parts of styrene, 2-5 parts of acrylic acid and 2-5 parts of acetoacetylated modified acrylic acid self-crosslinking monomer into a reaction kettle A, and dispersing and mixing at a high speed of 1000r/min for 20-40min to prepare a pre-emulsion A;
step two, preparation of organosilicon pre-emulsion B
Adding 100-120 parts of the pre-emulsion A obtained in the step one and 2-4 parts of vinyl triisopropoxysilane into a reaction kettle B, and dispersing and mixing at a high speed of 1000r/min for 20-40min to obtain an organic silicon pre-emulsion B;
step three, seed emulsion preparation
Adding 200-260 parts of deionized water, 10-20 parts of the pre-emulsion A obtained in the step one, 0.05-0.1 part of potassium persulfate and 0.4-0.6 part of sodium bicarbonate into a reaction kettle C, heating to 80-85 ℃, stirring at 200r/min for heat preservation and reacting until the solution presents blue light;
step four, emulsion polymerization
Controlling the temperature of the reaction kettle C to be 80-85 ℃, simultaneously dropwise adding a potassium persulfate aqueous solution and the residual pre-emulsion A in the second step into the reaction kettle C, continuously dropwise adding an organic silicon pre-emulsion B after the dropwise adding of the pre-emulsion A is finished, keeping the potassium persulfate aqueous solution and the pre-emulsion A and the organic silicon pre-emulsion B to be simultaneously dropwise added, completing the dropwise adding of the potassium persulfate aqueous solution and the organic silicon pre-emulsion B, heating to 85-90 ℃ after the dropwise adding is finished, preserving the heat for 2-3 hours, then cooling to 65-70 ℃, adding 0.2-0.5 part of tert-butyl hydroperoxide and 0.2-0.5 part of sodium erythorbate, and preserving the heat for 0.5-1 hour;
step five, compounding the emulsion
And (3) cooling the reaction kettle C to room temperature, adding the cohesion accelerator SA500, the preservative MV and the aqueous defoaming agent, adjusting the pH value to 7-8 by using ammonia water, adding the associative thickener, and uniformly stirring to obtain the organic silicon modified acrylate bedplate glue.
Further, the synthetic thickener is FS-300H produced by Liaoning sidereal fine chemical Co.
Further, the anionic emulsifier is an anionic surfactant novelusion ZS37A produced by Shanghai Zhiping Kogyo Co.
Further, in the fourth step, the potassium persulfate is kept to be simultaneously dripped with the pre-emulsion A and the organosilicon pre-emulsion B, and the time for finishing dripping the potassium persulfate is 2-4 hours.
Further, the potassium persulfate aqueous solution in the fourth step is prepared from the following raw materials in percentage by mass: 1-2 parts of potassium persulfate and 20-30 parts of deionized water.
Furthermore, in the fourth step, 0.2-0.5 part by weight of tert-butyl hydroperoxide and 0.2-0.5 part by weight of sodium erythorbate are added.
Further, in the fifth step, the weight parts of the components are as follows: the adhesive comprises, by weight, 0.5-1 part of cohesive force promoter SA 5000.5-1 part, 0.1-0.2 part of preservative MV, 0.5-1 part of associative thickener and 0.1-0.2 part of water-based defoamer.
Further, the organic silicon modified acrylate bedplate glue is prepared by the method.
The invention has the following advantages:
according to the invention, by adding vinyl triisopropoxysilane and introducing organosilicon into a polymer chain segment, wherein a molecular chain of the organosilicon has Si-O-Si bonds, and after adding a silane coupling agent into an acrylate emulsion, the Si-O-Si forms a stable cross-linked network structure, so that the cross-linking density can be improved, and a continuous and compact emulsion film can be formed; meanwhile, the Si-O-Si bond has excellent hydrophobic property, and can be enriched on the surface of a glue film when forming the film, so that the permeation of water molecules is hindered to a certain extent, and the silicon-based composite material has good moisture resistance after forming the film; the vinyl triisopropoxysilane is extremely easy to self-polymerize under the acidic condition, so the invention increases the usage amount of sodium bicarbonate as a buffering agent, controls the pH value of the reaction to be 4-5, simultaneously, dropwise adds the pre-emulsion containing the vinyl triisopropoxysilane in the latter half of the reaction, also effectively controls the self-polymerization of the silane coupling agent, simultaneously, the unique structure of the silane enables the silane to have very good stability in an aqueous system, and the silane can not react or crosslink before the emulsion is coagulated into a film, thereby ensuring the thermal stability of the emulsion.
The invention adopts the acetoacetylated modified acrylic acid self-crosslinking monomer (TAM) to replace N-hydroxymethyl acrylamide (NMA) as a crosslinking agent, solves the problem of continuous release of formaldehyde in the use process, simultaneously replaces acetoacetic acid ethylene glycol diester (AAEM), has more TAM and AAEM than molecular structure CH3, so the yellowing resistance is stronger, and simultaneously, due to the existence of more CH3, the high temperature resistance of the high polymer after film forming and crosslinking is also obviously improved.
The invention adopts the cohesion promoter SA500, is based on a special acrylate high-molecular emulsion product, is applied to a water-based acrylate pressure-sensitive adhesive system, can interact with an acrylic acid high-molecular chain for butyl acrylate system pressure-sensitive adhesives, and improves the cohesion of the emulsion in a small addition amount, thereby improving the strength and the heat resistance of the emulsion and hardly influencing the initial adhesion and the peeling strength of the emulsion.
The invention optimizes the type of the emulsifier, reduces the dosage of the emulsifier while reducing the gel fraction of the product, improves the stability of the emulsion, reduces the size of polymer particles by adopting the high-performance emulsifier, effectively achieves high viscosity without adding tackifying resin, and simultaneously effectively reduces the possibility of self-polymerization of the silane coupling agent.
The invention properly adds the isooctyl acrylate as a soft monomer, reduces the glass transition temperature, improves the initial adhesion force of the bedplate glue, adopts styrene as a hard monomer, and properly adds the styrene into the bedplate glue emulsion, thereby not greatly influencing the initial adhesion of the emulsion although the glass transition temperature is improved, and having obvious effects of high temperature and high humidity resistance and no back adhesion of the bedplate glue.
Therefore, the product has better moisture resistance, excellent thermal stability, higher yellowing resistance and high temperature resistance, and the emulsion has higher strength and heat resistance and has the capability of high viscosity but no anti-viscosity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
Fig. 1 is a test of the water-whitening resistance of the HF aqueous table glue and example 2 provided by the present invention, wherein a is the test result of the water-whitening resistance of example 2, and B is the test result of the water-whitening resistance of the HF aqueous table glue.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. 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.
Anionic emulsifiers anionic surfactants novelusion ZS37A, manufactured by shanghai zhiping limited;
SA500 produced by Dalianjindingxiang chemical Co., Ltd as cohesion accelerator;
USI-403 is produced by Tissui chemical Co., Ltd, Nanjing, Hessilication chemical Co., Ltd, vinyl triisopropoxysilane;
the acetoacetylated modified acrylic acid self-crosslinking monomer TAM is cured at room temperature by Beijing Baiyuan chemical Co., Ltd;
BY-706 manufactured BY antifoaming agent Beijing Baiyuan chemical Co., Ltd;
FS-300H is produced by Liaoning sidereal fine chemical Co.
Example 1
The preparation method of the silicone modified acrylate platen glue provided by the embodiment comprises the following steps:
step one, preparing pre-emulsion A
100kg of deionized water, 4kg of anionic emulsifier, 140kg of butyl acrylate, 100kg of isooctyl acrylate, 20kg of methyl methacrylate, 10kg of styrene, 2kg of acrylic acid and 2kg of acetoacetylated modified acrylic acid self-crosslinking monomer are added into a reaction kettle A, and the mixture is dispersed at a high speed of 900r/min for 30min to prepare 378kg of pre-emulsion A;
step two, preparation of organosilicon pre-emulsion B
Adding 100kg of the pre-emulsion A prepared in the step one into a reaction kettle B, adding 2kg of vinyl triisopropoxysilane, and dispersing at a high speed of 900r/min for 30min to obtain 102kg of organosilicon pre-emulsion B;
step three, seed emulsion preparation
Adding 240kg of deionized water, 20kg of the pre-emulsion A obtained in the step one, 0.1kg of potassium persulfate and 0.6kg of sodium bicarbonate into a reaction kettle C, heating to 80 ℃, stirring at 200r/min, and carrying out heat preservation reaction until the emulsion presents blue light;
step four, emulsion polymerization
Controlling the temperature of a reaction kettle C to be 80-85 ℃, and simultaneously dropwise adding a potassium persulfate aqueous solution and 278kg of the rest pre-emulsion A into the reaction kettle C, wherein the potassium persulfate aqueous solution is prepared from 1.2kg of potassium persulfate and 20kg of deionized water, after the pre-emulsion A is dropwise added, continuously dropwise adding an organic silicon pre-emulsion B, after the dropwise adding is completed within 3 hours, keeping the potassium persulfate aqueous solution and the pre-emulsion A and the organic silicon pre-emulsion B to be dropwise added simultaneously, and simultaneously completing the dropwise adding of the potassium persulfate aqueous solution and the organic silicon pre-emulsion B. After the dropwise adding, heating to 85 ℃, preserving the heat for 2 hours, then cooling to 65 ℃, adding 0.3kg of tert-butyl hydroperoxide and 0.3kg of sodium erythorbate, and preserving the heat for 0.5 hours;
step five, compounding the emulsion
After the temperature of the reaction kettle C is reduced to room temperature, adding the cohesion accelerator SA5000.5kg; preservative MV0.1 kg; 0.1kg of aqueous defoaming agent, adjusting the pH value to 7-8 with ammonia water, adding 0.5kg of associative thickener, and stirring uniformly to obtain the organic silicon modified acrylate plate glue product A.
Example 2
The preparation method of the silicone modified acrylate platen glue provided by the embodiment comprises the following steps:
step one, preparing pre-emulsion A
Adding 110kg of deionized water, 3kg of anionic emulsifier, 130kg of butyl acrylate, 110kg of isooctyl acrylate, 25kg of methyl methacrylate, 15kg of styrene, 2.5kg of acrylic acid and 2.5kg of acetoacetylated modified acrylic acid self-crosslinking monomer into a reaction kettle A, and dispersing at a high speed of 850r/min for 30min to prepare 398kg of pre-emulsion A;
step two, preparation of organosilicon pre-emulsion B
Adding 110kg of pre-emulsion A into a reaction kettle B, adding 2.5kg of vinyl triisopropoxysilane, and dispersing at 850r/min for 30min at a high speed to obtain 112.5kg of organosilicon pre-emulsion B;
step three, seed emulsion preparation
Adding 250kg of deionized water, 15kg of the pre-emulsion A obtained in the step 1, 0.1kg of potassium persulfate and 0.5kg of sodium bicarbonate into a reaction kettle C, heating to 80 ℃, stirring at 180r/min, and carrying out heat preservation reaction until the emulsion presents blue light;
step four, emulsion polymerization
Controlling the temperature of a reaction kettle C to be 80-85 ℃, and simultaneously dropwise adding a potassium persulfate aqueous solution and 288kg of the rest pre-emulsion A into the reaction kettle C, wherein the potassium persulfate aqueous solution is prepared from 1.5kg of potassium persulfate and 25kg of deionized water, continuously dropwise adding an organic silicon pre-emulsion B after the dropwise adding of the pre-emulsion A is finished, keeping the dropwise adding of the potassium persulfate aqueous solution and the pre-emulsion A and the dropwise adding of the organic silicon pre-emulsion B respectively after the dropwise adding of the pre-emulsion A is finished for 3 hours, and simultaneously finishing the dropwise adding of the potassium persulfate aqueous solution and the organic silicon. After the dropwise addition, the temperature is raised to 85 ℃, the temperature is kept for 2 hours, then the temperature is lowered to 65 ℃, 0.2kg of tert-butyl hydroperoxide and 0.2kg of sodium erythorbate are added, and the temperature is kept for 0.5 hours;
step five, compounding the emulsion
Cooling the reaction kettle C to room temperature, and adding a cohesion accelerator SA5000.7kg; preservative MV0.1 kg; 0.2kg of aqueous defoaming agent, adjusting the pH value to 7-8 with ammonia water, then adding 0.7kg of associative thickener, and stirring uniformly to obtain the organosilicon modified acrylate plate glue product B.
Example 3
The preparation method of the silicone modified acrylate platen glue provided by the embodiment comprises the following steps:
step one, preparing pre-emulsion A
Adding 120kg of deionized water, 5kg of anionic emulsifier, 160kg of butyl acrylate, 100kg of isooctyl acrylate, 30kg of methyl methacrylate, 10kg of styrene, 3kg of acrylic acid and 3kg of acetoacetylated modified acrylic acid self-crosslinking monomer into a reaction kettle A, and dispersing at a high speed of 1000r/min for 25min to obtain 430kg of pre-emulsion A;
step two, preparation of organosilicon pre-emulsion B
Adding 120kg of the pre-emulsion A into a reaction kettle B, adding 3kg of vinyl triisopropoxysilane, and dispersing at a high speed of 1000r/min for 25min to obtain 123kg of organosilicon pre-emulsion B;
step three, seed emulsion preparation
Adding 240kg of deionized water, 15kg of the pre-emulsion A obtained in the step 1, 0.07kg of potassium persulfate and 0.5kg of sodium bicarbonate into a reaction kettle C, heating to 80 ℃, stirring at 200r/min, and carrying out heat preservation reaction until the emulsion presents blue light;
step four, emulsion polymerization
Controlling the temperature of a reaction kettle C to be 80-85 ℃, and simultaneously dropwise adding a potassium persulfate aqueous solution and 310kg of the rest pre-emulsion A into the reaction kettle C, wherein the potassium persulfate aqueous solution is prepared from 1.4kg of potassium persulfate and 20kg of deionized water, continuously dropwise adding an organic silicon pre-emulsion B after the dropwise adding of the pre-emulsion A is finished, keeping the dropwise adding of the potassium persulfate aqueous solution and the pre-emulsion A and the dropwise adding of the organic silicon pre-emulsion B respectively after the dropwise adding of the pre-emulsion A is finished for 3 hours, and simultaneously finishing the dropwise adding of the potassium persulfate aqueous solution and the organic silicon. After the dropwise addition, the temperature is raised to 85 ℃, the temperature is kept for 2 hours, then the temperature is lowered to 65 ℃, 0.4kg of tert-butyl hydroperoxide and 0.4kg of sodium erythorbate are added, and the temperature is kept for 0.5 hour;
step five, compounding the emulsion
When the temperature of the reaction kettle C is reduced to the room temperature, SA5000.5kg of cohesion accelerator is added; preservative MV 0.2 kg; 0.2kg of aqueous defoaming agent, adjusting the pH value to 7-8 with ammonia water, adding 0.7kg of associative thickener, and stirring uniformly to obtain the organic silicon modified acrylate plate glue product C.
Example 4
The preparation method of the silicone modified acrylate platen glue provided by the embodiment comprises the following steps:
step one, preparing pre-emulsion A
100kg of deionized water, 4.5kg of anionic emulsifier, 120kg of butyl acrylate, 120kg of isooctyl acrylate, 20kg of methyl methacrylate, 15kg of styrene, 2kg of acrylic acid and 4kg of acetoacetylated modified acrylic acid self-crosslinking monomer are added into a reaction kettle A, and the mixture is dispersed at a high speed of 900r/min for 30min to prepare 385.5kg of pre-emulsion A;
step two, preparation of organosilicon pre-emulsion B
Adding 110kg of the pre-emulsion A in the reaction kettle A into the reaction kettle B, adding 2kg of vinyl triisopropoxysilane into the reaction kettle B, and dispersing at a high speed of 900r/min for 30min to obtain 112kg of organosilicon pre-emulsion B;
step three, seed emulsion preparation
Adding 250kg of deionized water, 20kg of the pre-emulsion A obtained in the step (1), 0.05kg of potassium persulfate and 0.6kg of sodium bicarbonate into a reaction kettle C, heating to 80 ℃, stirring at 200r/min, and carrying out heat preservation reaction until the emulsion presents blue light;
step four, emulsion polymerization
Controlling the temperature of a reaction kettle C to be 80-85 ℃, and simultaneously dripping a potassium persulfate aqueous solution and 275.5kg of the rest pre-emulsion A into the reaction kettle C, wherein the potassium persulfate aqueous solution is prepared by 1.5kg of potassium persulfate and 25kg of deionized water, the organic silicon pre-emulsion B is continuously dripped after the dripping of the pre-emulsion A is finished, the dripping is finished within 3 hours, the potassium persulfate aqueous solution is respectively dripped simultaneously with the pre-emulsion A and the organic silicon pre-emulsion B, and the dripping of the potassium persulfate aqueous solution and the organic silicon pre-emulsion B is finished simultaneously. After the dropwise addition, the temperature is raised to 85 ℃, the temperature is kept for 2 hours, then the temperature is lowered to 65 ℃, 0.2kg of tert-butyl hydroperoxide and 0.2kg of sodium erythorbate are added, and the temperature is kept for 1 hour;
step five, compounding the emulsion
After the temperature of the reaction kettle C is reduced to room temperature, adding the cohesion accelerator SA5000.5kg; preservative MV0.1 kg; 0.1kg of aqueous defoaming agent, adjusting the pH value to 7-8 with ammonia water, adding 0.5kg of associative thickener, and stirring uniformly to obtain the organosilicon modified acrylate plate glue product D.
Example 5
The preparation method of the silicone modified acrylate platen glue provided by the embodiment comprises the following steps:
step one, preparing pre-emulsion A
Adding 120kg of deionized water, 4kg of anionic emulsifier, 150kg of butyl acrylate, 110kg of isooctyl acrylate, 20kg of methyl methacrylate, 15kg of styrene, 2kg of acrylic acid and 2kg of acetoacetylated modified acrylic acid self-crosslinking monomer into a reaction kettle A, and dispersing at a high speed of 900r/min for 30min to obtain a pre-emulsion A423 kg;
step two, preparation of organosilicon pre-emulsion B
100kg of the pre-emulsion A in the reaction kettle A is added into a reaction kettle B, 2kg of vinyl triisopropoxysilane is added, and the mixture is dispersed at a high speed of 900r/min for 30min to obtain 102kg of organosilicon pre-emulsion B;
step three, seed emulsion preparation
Adding 260kg of deionized water, 20kg of the pre-emulsion A obtained in the step 1, 0.1kg of potassium persulfate and 0.6kg of sodium bicarbonate into a reaction kettle C, heating to 80 ℃, stirring at 200r/min, and carrying out heat preservation reaction until the emulsion presents blue light;
step four, emulsion polymerization
Controlling the temperature of a reaction kettle C to be 80-85 ℃, and simultaneously dropwise adding a potassium persulfate aqueous solution and 323kg of the rest pre-emulsion A into the reaction kettle C, wherein the potassium persulfate aqueous solution is prepared from 1.3kg of potassium persulfate and 25kg of deionized water, continuously dropwise adding an organic silicon pre-emulsion B after the dropwise adding of the pre-emulsion A is finished, keeping the dropwise adding of the potassium persulfate aqueous solution and the pre-emulsion A and the dropwise adding of the organic silicon pre-emulsion B respectively after the dropwise adding of the pre-emulsion A is finished for 3 hours, and simultaneously finishing the dropwise adding of the potassium persulfate aqueous solution and the organic silicon. After the dropwise addition, the temperature is raised to 85 ℃, the temperature is kept for 2 hours, then the temperature is lowered to 65 ℃, 0.3kg of tert-butyl hydroperoxide and 0.3kg of sodium erythorbate are added, and the temperature is kept for 1 hour;
step five, compounding the emulsion
After the temperature of the reaction kettle C is reduced to room temperature, adding the cohesion accelerator SA5000.5kg; preservative MV0.1 kg; 0.1kg of aqueous defoaming agent, adjusting the pH value to 7-8 with ammonia water, adding 0.5kg of associative thickener, and stirring uniformly to obtain the organic silicon modified acrylate plate glue product E.
Test example
The organic silicon modified acrylate platen glue products of the embodiments 1-5 and the HF aqueous platen glue sold in the comparative example (manufactured by Weir Fine chemical Co., Ltd., Jiangshan city) are dried by hot air with the thickness of each layer being 25 μm on a platen of an elliptical machine by a blade coating tool, blade coating is continuously carried out for three times, the cloth cover temperature is kept at 40 ℃ on the elliptical machine, the indoor humidity is higher than 60%, and the test can be carried out after the platen glue is completely dried.
1. Initial adhesion test
The test was performed according to GB/T4852-2002.
2. High temperature permanent adhesion test
The test was performed according to GB/T4851-1998.
3. Water whitening resistance test
The polyacrylate emulsion was spread on a platen with an applicator, a drop of soapy water was applied, a timer was started, and after 30 minutes, the pressure sensitive adhesive was observed to whiten as shown in fig. 1.
4. Return test
The pure cotton knitted fabric is laid on an elliptical machine, the cloth cover temperature is kept at 40 ℃, the indoor humidity is higher than 60%, after ironing is carried out by using an iron, printing and drying are carried out on the cotton fabric, the cotton fabric is immediately uncovered, and the table board glue is judged whether or not on the back surface of the cotton fabric or the amount of the table board glue stuck up is judged.
Table 1 comparative results of test examples table
The test result shows that compared with the table plate glue and the market sample, the table plate glue has higher initial adhesion, high-temperature permanent adhesion, water white resistance, no return to the table, better high-temperature and high-humidity resistance and low 180-degree peel strength, but cloth is easier to take after printing is finished, so the table plate glue is superior to the sample in various performances, and the product is safe and environment-friendly and has better market prospect.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. The preparation method of the organic silicon modified acrylate bedplate glue is characterized by comprising the following steps of:
step one, preparation of pre-emulsion A
Adding 100-120 parts of deionized water, 4-5 parts of an anionic emulsifier, 120-160 parts of butyl acrylate, 80-120 parts of isooctyl acrylate, 20-30 parts of methyl methacrylate, 10-20 parts of styrene, 2-5 parts of acrylic acid and 2-5 parts of acetoacetylated modified acrylic acid self-crosslinking monomer into a reaction kettle A, and dispersing and mixing at a high speed of 1000r/min for 20-40min to prepare a pre-emulsion A;
step two, preparation of organosilicon pre-emulsion B
Adding 100-120 parts of the pre-emulsion A obtained in the step one and 2-4 parts of vinyl triisopropoxysilane into a reaction kettle B, and dispersing and mixing at a high speed of 1000r/min for 20-40min to obtain an organic silicon pre-emulsion B;
step three, seed emulsion preparation
Adding 200-260 parts of deionized water, 10-20 parts of the pre-emulsion A obtained in the step one, 0.05-0.1 part of potassium persulfate and 0.4-0.6 part of sodium bicarbonate into a reaction kettle C, heating to 80-85 ℃, stirring at 200r/min for heat preservation and reacting until the emulsion presents blue light;
step four, emulsion polymerization
Controlling the temperature of a reaction kettle C to be 80-85 ℃, simultaneously dropwise adding a potassium persulfate aqueous solution and the rest of pre-emulsion A into the reaction kettle C, continuously dropwise adding an organic silicon pre-emulsion B after the pre-emulsion A is dropwise added, keeping the potassium persulfate aqueous solution and the pre-emulsion A and the organic silicon pre-emulsion B to be dropwise added simultaneously, completing the dropwise adding of the potassium persulfate aqueous solution and the organic silicon pre-emulsion B simultaneously, heating to 85-90 ℃ after the dropwise adding is completed, preserving the heat for 2-3 hours, then cooling to 65-70 ℃, adding 0.2-0.5 part of tert-butyl hydroperoxide and 0.2-0.5 part of sodium isoascorbate, and preserving the heat for 0.5-1 hour;
step five, compounding the emulsion
And (3) cooling the reaction kettle C to room temperature, adding the cohesion accelerator SA500, the preservative MV and the aqueous defoaming agent, adjusting the pH value to 7-8 by using ammonia water, adding the associative thickener, and uniformly stirring to obtain the organic silicon modified acrylate bedplate glue.
2. The method for preparing the silicone modified acrylate platen gum according to claim 1,
the synthetic thickener is FS-300H produced by Liaoning sidereal fine chemical Co.
3. The method for preparing the silicone modified acrylate platen gum according to claim 1,
the anionic emulsifier is an anionic surfactant novelusion ZS37A produced by Shanghai Zhiping Kogyo Co.
4. The method for preparing the silicone modified acrylate platen gum according to claim 1,
and in the fourth step, the potassium persulfate is kept to be simultaneously dripped with the pre-emulsion A and the organic silicon pre-emulsion B respectively, and the time for finishing dripping the potassium persulfate is 2-4 h.
5. The method for preparing the silicone modified acrylate platen gum according to claim 1,
the potassium persulfate aqueous solution in the fourth step is prepared from the following raw materials in parts by weight: 1-2 parts of potassium persulfate and 20-30 parts of deionized water.
6. The method for preparing the silicone modified acrylate platen gum according to claim 1,
in the fourth step, 0.2-0.5 part by weight of tert-butyl hydroperoxide and 0.2-0.5 part by weight of sodium erythorbate are added.
7. The method for preparing the silicone modified acrylate platen gum according to claim 1,
in the fifth step, the weight parts of the components are as follows: the adhesive comprises, by weight, 0.5-1 part of cohesive force promoter SA 5000.5-1 part, 0.1-0.2 part of preservative MV, 0.5-1 part of associative thickener and 0.1-0.2 part of water-based defoamer.
8. A silicone modified acrylate size prepared by the process of claims 1-7.
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