CN110951428A - APEO-free acrylate electrostatic flocking adhesive and preparation method thereof - Google Patents
APEO-free acrylate electrostatic flocking adhesive and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/08—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/10—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses an APEO-free acrylate electrostatic flocking adhesive which comprises the following components in percentage by mass: 10-20 wt.% of epoxy resin E4410, 5-15 wt.% of KH580 silane coupling agent, 5-5 wt.% of non-ionic emulsifier A-9802.5, 0.5-1 wt.% of sodium dodecyl sulfate, 10-15 wt.% of butyl methacrylate, 10-15 wt.% of isooctyl acrylate, 0.5-2 wt.% of diacetone acrylamide, 0.2-2 wt.% of adipic dihydrazide, 0.5-2 wt.% of acrylic acid, 0.4-1 wt.% of potassium persulfate, 1-10 wt.% of nano antimony trioxide powder and 10-55 wt.% of deionized water. The invention also discloses a preparation method of the adhesive for electrostatic flocking. The adhesive is used in a flocking process, can endow textiles with excellent high temperature resistance, chemical resistance, ultraviolet light resistance, flame retardance and the like, has good solvent resistance, is green and environment-friendly, has high bonding strength, and has good bonding force on fluff and cloth. In addition, the product has good stability and long storage period, and can be stored for more than 1 year in a sealed manner at normal temperature.
Description
Technical Field
The invention belongs to the technical field of electrostatic flocking fabrics, and particularly relates to an APEO-free acrylate electrostatic flocking adhesive and a preparation method thereof.
Background
The electrostatic flocking comprises a substrate, an adhesive and fluff, which are commonly called as three major parts, wherein the adhesive on the surface of the substrate is the key for influencing the quality of electrostatic flocking products, and the performance of the electrostatic flocking products directly determines the flocking fastness and the handfeel of the flocking products.
The adhesive used in the electrostatic flocking process is acrylate adhesive which accounts for more than 90% of the adhesive used for flocking, has good film forming property, flexibility, ageing resistance, weather resistance and excellent mechanical property, and is environment-friendly and widely applied in the preparation and use processes. However, the adhesive has some inherent defects, which affect the normal performance of the adhesive, and mainly comprises the following aspects:
(1) the acrylic acid adhesive has the defects of wear resistance, hand feeling, wet fastness and the like;
(2) the main chain structure and the side group of the acrylic resin seriously restrict the performance of the acrylic resin, so that the adhesive has poor water resistance, becomes brittle at low temperature, becomes sticky at high temperature, loses the original strength and has poor weather resistance;
(3) the film formed by the acrylic acid adhesive is easy to swell under the action of an organic solvent, so that the coating falls off; in the electrostatic flocking process, the hand feeling and the flocking fastness are seriously influenced by the using amount of the adhesive, and the contradiction is difficult to solve;
(4) the traditional acrylic acid adhesive needs to be cured at a higher temperature (140-150 ℃) to form a film, which is mainly caused by the fact that N-methylolacrylamide (NMA) crosslinking monomer is commonly used in the adhesive, so that the energy consumption problem is caused, and the requirements of energy conservation and environmental protection are not met.
Therefore, in order to solve the above problems, it is necessary to modify the acrylic adhesive, for example, acrylate modified by silicone and epoxy resin has not only its own characteristics but also the characteristics of silicone and epoxy resin. Because the main chain structure of the organic silicon resin contains Si-O bonds with high bond energy (the bond energy is up to 450 kJ/mol), the resin has excellent performances of high temperature resistance, chemical resistance, ultraviolet light resistance and the like, and simultaneously, the resin has lower surface energy and is endowed with excellent water resistance and stain resistance. The structural characteristics of the epoxy resin determine that the polymer after reaction has the characteristics of high cohesive force, strong adhesive force and good solvent resistance.
In addition, alkylphenol ethoxylates (APEO) and its derivatives are frequently used as emulsifiers in the preparation of acrylic adhesives, which causes problems in that the APEO content in the adhesives is too high, and the APEO has serious effects on the ecological environment, including toxicity, biodegradability, environmental hormones, and the generation of harmful by-products in actual production. Therefore, since some european countries have enacted corresponding regulations restricting the production and use of APEO since the last 70 th century, where the APEO content of textiles and garments exported to europe is allowed to not exceed 0.1%, it is the first problem to solve the APEO content in emulsifiers for the production of high value-added electrostatic flocking products.
Disclosure of Invention
The invention aims to solve the problems in the prior art, provides an APEO-free acrylate electrostatic flocking adhesive and a preparation method thereof, and the obtained adhesive is applied to an electrostatic flocking process to endow textiles with excellent high temperature resistance, chemical resistance, ultraviolet light resistance and other performances, and the adhesive is high in bonding strength, good in solvent resistance and good in flame retardance.
The invention adopts the technical scheme that an APEO-free acrylate electrostatic flocking adhesive comprises the following raw materials in percentage by mass: 10-20 wt.% of epoxy resin E4410, 5-15 wt.% of KH580 silane coupling agent, 5-5 wt.% of non-ionic emulsifier A-9802.5, 0.5-1 wt.% of sodium dodecyl sulfate, 10-15 wt.% of butyl methacrylate, 10-15 wt.% of isooctyl acrylate, 0.5-2 wt.% of diacetone acrylamide, 0.2-2 wt.% of adipic dihydrazide, 0.5-2 wt.% of acrylic acid, 0.4-1 wt.% of potassium persulfate, 1-10 wt.% of nano antimony trioxide powder and 10-55 wt.% of deionized water.
A method of preparing an APEO-free acrylate electrostatic flocking adhesive comprising the steps of:
(1) preparation of the Pre-emulsion
Adding the nonionic emulsifier A-980, sodium dodecyl sulfate and part of deionized water into a pre-emulsifying kettle, stirring, fully dissolving at the stirring speed of 800-1000 rpm, then adding the epoxy resin E44, butyl methacrylate, isooctyl acrylate, diacetone acrylamide and acrylic acid monomer into the pre-emulsifying kettle, and fully stirring to obtain the pre-emulsion.
(2) Preparation of epoxy resin/organic silicon composite modified acrylate emulsion
Adding part of the pre-emulsion into a reaction kettle, sequentially adding the rest deionized water and part of the initiator, adjusting the temperature to 70-80 ℃, reacting for 0.5-1 h, then starting the emulsion to show blue light, continuously dropwise adding the pre-emulsion and the initiator, controlling the reaction temperature to be 75-85 ℃, controlling the dropwise adding time to be 2.5-3 h, when all the pre-emulsion is dripped off and the initiator remains, dripping KH580 and the remaining initiator into the reaction kettle, controlling the dripping time to be between 0.5 and 1 hour, keeping the reaction temperature to be between 75 and 85 ℃, keeping the reaction time to be 0.5 to 1 hour, adjusting the temperature to be between 80 and 90 ℃ after the reaction, curing for 1 hour, then cooling to 30-40 ℃, adjusting the pH value to 7-9 by ammonia water, adding adipic dihydrazide, stirring for 15min, filtering and discharging to obtain the epoxy resin/organic silicon composite modified acrylate emulsion.
(3) Preparation of APEO-free acrylate electrostatic flocking adhesive
And (3) adding the epoxy resin/organic silicon composite modified acrylate emulsion prepared in the step (2) and nano antimony trioxide powder into a common plastic tank for stirring, wherein the stirring speed is 800-1000 r/min, and after stirring for 20-30 min, adjusting the solid content of the emulsion to 40-50 wt% by using a proper amount of deionized water to obtain the product.
The ammonia water for adjusting the pH value is not in the range of the raw materials.
The deionized water used for adjusting the solid content is not in the range of the deionized water in the raw material proportion.
Further, the mass ratio of the nonionic emulsifier A-980 to the sodium dodecyl sulfate in the step (1) is 5: 1.
Further, in the step (2), any one of KH550, KH560 and KH590 can be used as the KH580 silane coupling agent.
Further, the amount of the adipic acid dihydrazide used in the step (2) is 1/2 which is the amount of the diacetone acrylamide substance.
Further, the nano antimony trioxide powder in the step (3) can be replaced by any one of nano aluminum oxide and nano magnesium oxide.
Further, the mass ratio of the epoxy resin/organic silicon composite modified acrylate emulsion and the nano antimony trioxide powder in the step (3) is 10: 1.
Furthermore, the mass ratio of the epoxy resin/organic silicon composite modified acrylate emulsion to the nano aluminum oxide is 10: 1.
Furthermore, the mass ratio of the epoxy resin/organic silicon composite modified acrylate emulsion to the nano magnesium oxide is 10: 1.
By adopting the technical scheme provided by the invention, the following beneficial effects can be obtained:
(1) the adhesive prepared by the invention endows the textile with excellent performances of high temperature resistance, chemical resistance, ultraviolet light resistance and the like, has good solvent resistance, is green and environment-friendly, has high bonding strength, and has good bonding force on fluff and cloth.
(2) Because the flame-retardant nano material is added in the adhesive formula, the prepared flocking product has better flame retardant property.
(3) The adhesive prepared by the invention has good stability and long storage period, and can be stored for more than 1 year in a sealing way at normal temperature.
The specific implementation mode is as follows:
the present invention will be further described with reference to the following specific examples.
Example 1:
an APEO-free acrylate electrostatic flocking adhesive comprises the following raw materials in percentage by mass: epoxy resin E4410 wt%, KH580 silane coupling agent 5%, non-ionic emulsifier a-9802.5%, sodium lauryl sulfate 0.5%, butyl methacrylate 10%, isooctyl acrylate 10%, diacetone acrylamide 0.5%, adipic dihydrazide 0.26%, acrylic acid 0.5%, potassium persulfate 0.4%, nano antimony trioxide powder 10%, and deionized water 50.34%.
A method of preparing an APEO-free acrylate electrostatic flocking adhesive comprising the steps of:
(1) preparation of the Pre-emulsion
Adding a nonionic emulsifier A-980, sodium dodecyl sulfate and deionized water accounting for 40-50 wt.% of the total weight of water into a pre-emulsifying kettle, stirring, fully dissolving at the stirring speed of 800-1000 rpm, then adding epoxy resin E44, butyl methacrylate, isooctyl acrylate, diacetone acrylamide and acrylic acid monomers into the pre-emulsifying kettle, and fully stirring to obtain a pre-emulsion.
(2) Preparation of epoxy resin/organic silicon composite modified acrylate emulsion
1/5 (by weight) of the pre-emulsion is added into a reaction kettle, 1/5 (by weight) of the rest deionized water and the rest initiator is sequentially added, the temperature is adjusted to 70-80 ℃, the emulsion begins to present blue light after 0.5-1 h of reaction, the pre-emulsion and the initiator are continuously dripped, the reaction temperature is controlled to be 75-85 ℃, the dripping time is controlled to be 2.5-3 h, when the pre-emulsion is completely dripped and the rest initiator remains, KH580 and the rest initiator are dripped into the reaction kettle, the dripping time is controlled to be 0.5-1 h, the reaction temperature is still kept to be 75-85 ℃, the reaction time is 0.5-1 h, the temperature is adjusted to be 80-90 ℃ after the reaction, the mixture is cured for 1h, then the temperature is reduced to be 30-40 ℃, the pH value is adjusted to be 7-9 by ammonia water, adipic dihydrazide is added, the mixture is stirred for 15min, and the mixture is filtered and discharged, thus obtaining the epoxy resin/organic silicon composite modified acrylate emulsion.
(3) Preparation of APEO-free acrylate electrostatic flocking adhesive
And (3) adding the epoxy resin/organic silicon composite modified acrylate emulsion prepared in the step (2) and nano antimony trioxide powder into a common plastic tank for stirring, wherein the stirring speed is 800-1000 r/min, and after stirring for 20-30 min, adjusting the solid content of the emulsion to 40-50 wt% by using a proper amount of deionized water to obtain the product.
The ammonia water for adjusting the pH value is not in the range of the raw materials.
The deionized water used for adjusting the solid content is not in the range of the deionized water in the raw material proportion.
The mass ratio of the nonionic emulsifier A-980 to the sodium dodecyl sulfate in the step (1) is 5: 1.
The amount of the adipic acid dihydrazide used in the step (2) is 1/2 which is the amount of the diacetone acrylamide substance.
The mass ratio of the epoxy resin/organic silicon composite modified acrylate emulsion and the nano antimony trioxide powder in the step (3) is 10: 1.
Example 2:
an APEO-free acrylate electrostatic flocking adhesive comprises the following raw materials in percentage by mass: epoxy E4415 wt%, KH550 silane coupling agent 10%, non-ionic emulsifier a-9803.8%, sodium lauryl sulfate 0.76%, butyl methacrylate 12.5%, isooctyl acrylate 12.5%, diacetone acrylamide 1.25%, adipic dihydrazide 0.64%, acrylic acid 1.25%, potassium persulfate 0.7%, alumina powder 5.5%, and deionized water 36.1%.
A method of preparing an APEO-free acrylate electrostatic flocking adhesive comprising the steps of:
(1) preparation of the Pre-emulsion
Adding a nonionic emulsifier A-980, sodium dodecyl sulfate and deionized water accounting for 40-50 wt.% of the total weight of water into a pre-emulsifying kettle, stirring, fully dissolving at the stirring speed of 800-1000 rpm, then adding epoxy resin E44, butyl methacrylate, isooctyl acrylate, diacetone acrylamide and acrylic acid monomers into the pre-emulsifying kettle, and fully stirring to obtain a pre-emulsion.
(2) Preparation of epoxy resin/organic silicon composite modified acrylate emulsion
1/5 (by weight) of the pre-emulsion is added into a reaction kettle, 1/5 (by weight) of the rest deionized water and the rest initiator is sequentially added, the temperature is adjusted to 70-80 ℃, the emulsion begins to present blue light after 0.5-1 h of reaction, the pre-emulsion and the initiator are continuously dripped, the reaction temperature is controlled to be 75-85 ℃, the dripping time is controlled to be 2.5-3 h, when the pre-emulsion is completely dripped and the rest initiator remains, KH550 and the rest initiator are dripped into the reaction kettle, the dripping time is controlled to be 0.5-1 h, the reaction temperature is still kept to be 75-85 ℃, the reaction time is 0.5-1 h, the temperature is adjusted to be 80-90 ℃ after the reaction, the mixture is cured for 1h, then the temperature is reduced to be 30-40 ℃, the pH value is adjusted to be 7-9 by ammonia water, adipic dihydrazide is added, the mixture is stirred for 15min, and then the mixture is filtered and discharged, thus obtaining the epoxy resin/organic silicon composite modified acrylate emulsion.
(3) Preparation of APEO-free acrylate electrostatic flocking adhesive
And (3) stirring the epoxy resin/organic silicon composite modified acrylate emulsion prepared in the step (2) and nano-alumina powder in a common plastic tank at the stirring speed of 800-1000 rpm for 20-30 minutes, and then adjusting the solid content of the emulsion to 40-50 wt% by using a proper amount of deionized water to obtain the product.
The ammonia water for adjusting the pH value is not in the range of the raw materials.
The deionized water used for adjusting the solid content is not in the range of the deionized water in the raw material proportion.
The mass ratio of the nonionic emulsifier A-980 to the sodium dodecyl sulfate in the step (1) is 5: 1.
The amount of the adipic acid dihydrazide used in the step (2) is 1/2 which is the amount of the diacetone acrylamide substance.
The mass ratio of the epoxy resin/organic silicon composite modified acrylate emulsion to the nano alumina powder in the step (3) is 10: 1.
Example 3:
an APEO-free acrylate electrostatic flocking adhesive comprises the following raw materials in percentage by mass: epoxy E4410 wt%, KH560 silane coupling agent 10 wt%, non-ionic emulsifier a-9805 wt%, sodium lauryl sulfate 1 wt%, butyl methacrylate 15 wt%, isooctyl acrylate 10 wt%, diacetone acrylamide 2 wt%, adipic dihydrazide 1.03 wt%, acrylic acid 2 wt%, potassium persulfate 1 wt%, magnesium oxide powder 1 wt%, and deionized water 41.97 wt%.
A method of preparing an APEO-free acrylate electrostatic flocking adhesive comprising the steps of:
(1) preparation of the Pre-emulsion
Adding a nonionic emulsifier A-980, sodium dodecyl sulfate and deionized water accounting for 40-50 wt.% of the total weight of water into a pre-emulsifying kettle, stirring, fully dissolving at the stirring speed of 800-1000 rpm, then adding epoxy resin E44, butyl methacrylate, isooctyl acrylate, diacetone acrylamide and acrylic acid monomers into the pre-emulsifying kettle, and fully stirring to obtain a pre-emulsion.
(2) Preparation of epoxy resin/organic silicon composite modified acrylate emulsion
1/5 (by weight) of the pre-emulsion is added into a reaction kettle, 1/5 (by weight) of the rest deionized water and the rest initiator is sequentially added, the temperature is adjusted to 70-80 ℃, the emulsion begins to present blue light after 0.5-1 h of reaction, the pre-emulsion and the initiator are continuously dripped, the reaction temperature is controlled to be 75-85 ℃, the dripping time is controlled to be 2.5-3 h, when the pre-emulsion is completely dripped and the rest initiator remains, KH560 and the rest initiator are dripped into the reaction kettle, the dripping time is controlled to be 0.5-1 h, the reaction temperature is still kept to be 75-85 ℃, the reaction time is 0.5-1 h, the temperature is adjusted to be 80-90 ℃ after the reaction, the mixture is cured for 1h, then the temperature is reduced to be 30-40 ℃, the pH value is adjusted to be 7-9 by ammonia water, adipic dihydrazide is added, the mixture is stirred for 15min, and then the mixture is filtered and discharged, thus obtaining the epoxy resin/organic silicon composite modified acrylate emulsion.
(3) Preparation of APEO-free acrylate electrostatic flocking adhesive
And (3) adding the epoxy resin/organic silicon composite modified acrylate emulsion prepared in the step (2) and the nano magnesium oxide powder into a common plastic tank for stirring, wherein the stirring speed is 800-1000 r/min, and after stirring for 20-30 min, adjusting the solid content of the emulsion to 40-50 wt% by using a proper amount of deionized water to obtain the product.
The ammonia water for adjusting the pH value is not in the range of the raw materials.
The deionized water used for adjusting the solid content is not in the range of the deionized water in the raw material proportion.
The mass ratio of the nonionic emulsifier A-980 to the sodium dodecyl sulfate in the step (1) is 5: 1.
The amount of the adipic acid dihydrazide used in the step (2) is 1/2 which is the amount of the diacetone acrylamide substance.
The mass ratio of the epoxy resin/organic silicon composite modified acrylate emulsion and the nano magnesium oxide powder in the step (3) is 10: 1.
The adhesive prepared by the invention is used in a flocking process, can endow textiles with excellent high temperature resistance, chemical resistance, ultraviolet light resistance, flame retardance and the like, has good solvent resistance, is green and environment-friendly, has high bonding strength, and has good bonding force on fluff and cloth. In addition, the product has good stability and long storage period, and can be stored for more than 1 year in a sealed manner at normal temperature.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (7)
1. The APEO-free acrylate electrostatic flocking adhesive is characterized by comprising the following raw materials in percentage by mass: 10-20 wt.% of epoxy resin E4410, 5-15 wt.% of KH580 silane coupling agent, 5-5 wt.% of non-ionic emulsifier A-9802.5, 0.5-1 wt.% of sodium dodecyl sulfate, 10-15 wt.% of butyl methacrylate, 10-15 wt.% of isooctyl acrylate, 0.5-2 wt.% of diacetone acrylamide, 0.2-2 wt.% of adipic dihydrazide, 0.5-2 wt.% of acrylic acid, 0.4-1 wt.% of potassium persulfate, 1-10 wt.% of nano antimony trioxide powder and 10-55 wt.% of deionized water.
2. A method of preparing the APEO-free acrylate electrostatic flocking adhesive of claim 1 comprising the steps of:
(1) preparation of the Pre-emulsion
Adding a nonionic emulsifier A-980, sodium dodecyl sulfate and part of deionized water into a pre-emulsifying kettle, stirring, fully dissolving at the stirring speed of 800-1000 r/min, then adding epoxy resin E44, butyl methacrylate, isooctyl acrylate, diacetone acrylamide and acrylic acid monomers into the pre-emulsifying kettle, and fully stirring to obtain a pre-emulsion;
(2) preparation of epoxy resin/organic silicon composite modified acrylate emulsion
Adding part of the pre-emulsion into a reaction kettle, sequentially adding the rest deionized water and part of the initiator, adjusting the temperature to 70-80 ℃, reacting for 0.5-1 h, then starting the emulsion to show blue light, continuously dropwise adding the pre-emulsion and the initiator, controlling the reaction temperature to be 75-85 ℃, controlling the dropwise adding time to be 2.5-3 h, when all the pre-emulsion is dripped off and the initiator remains, dripping KH580 and the remaining initiator into the reaction kettle, controlling the dripping time to be between 0.5 and 1 hour, keeping the reaction temperature to be between 75 and 85 ℃, keeping the reaction time to be 0.5 to 1 hour, adjusting the temperature to be between 80 and 90 ℃ after the reaction, curing for 1 hour, then cooling to 30-40 ℃, adjusting the pH value to 7-9 by ammonia water, adding adipic dihydrazide, stirring for 15min, filtering and discharging to obtain epoxy resin/organic silicon composite modified acrylate emulsion;
(3) preparation of APEO-free acrylate electrostatic flocking adhesive
Adding the epoxy resin/organic silicon composite modified acrylate emulsion prepared in the step (2) and nano antimony trioxide powder into a common plastic tank for stirring, wherein the stirring speed is 800-1000 r/min, and after stirring for 20-30 min, adjusting the solid content of the emulsion to 40-50 wt% by using a proper amount of deionized water to obtain a product;
the ammonia water for adjusting the PH value is not in the range of the raw materials;
the deionized water used for adjusting the solid content is not in the range of the deionized water in the raw material proportion.
3. The method for preparing the APEO-free acrylate electrostatic flocking adhesive as claimed in claim 2, wherein the mass ratio of the nonionic emulsifier A-980 to the sodium lauryl sulfate in the step (1) is 5: 1.
4. The method for preparing the APEO-free acrylate electrostatic flocking adhesive as claimed in claim 2, wherein the KH580 silane coupling agent used in the step (2) is any one of KH550, KH560 and KH 590.
5. The method for preparing an APEO-free acrylate electrostatic flocking adhesive as claimed in claim 2, wherein the amount of the adipic acid dihydrazide used in the step (2) is 1/2 which is the amount of the diacetone acrylamide substance.
6. The method for preparing the APEO-free acrylate electrostatic flocking binder as claimed in claim 2, wherein the nano antimony trioxide powder in the step (3) is replaced by any one of nano aluminum oxide and nano magnesium oxide.
7. The method for preparing the APEO-free acrylate electrostatic flocking adhesive as claimed in any one of claims 2, 3, 4, 5 and 6, wherein the mass ratio of the epoxy resin/silicone composite modified acrylate emulsion and the nano antimony trioxide powder in step (3) is 10: 1;
or the mass ratio of the epoxy resin/organic silicon composite modified acrylate emulsion to the nano aluminum oxide powder is 10: 1;
or the mass ratio of the epoxy resin/organic silicon composite modified acrylate emulsion to the nano magnesium oxide powder is 10: 1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113637431A (en) * | 2021-08-30 | 2021-11-12 | 惠州市强茂化工科技有限公司 | Pressure-sensitive adhesive, pressure-sensitive adhesive layer, method for preparing pressure-sensitive adhesive and method for preparing pressure-sensitive adhesive layer |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423735A (en) * | 2008-12-05 | 2009-05-06 | 武汉科技学院 | Method for preparing environment-friendly type organosilicon modified acrylic ester binding agent |
| CN102174305A (en) * | 2010-12-14 | 2011-09-07 | 北京高盟新材料股份有限公司 | Acrylate adhesive for reflective cloth and preparation method thereof |
| CN103214993A (en) * | 2013-05-04 | 2013-07-24 | 辽宁恒星精细化工有限公司 | Acrylic ester electrostatic flocking binding agent and preparation method thereof |
| CN104015414A (en) * | 2014-06-18 | 2014-09-03 | 航天海鹰(镇江)特种材料有限公司 | Aerogel composite fabric utilizing aqueous adhesive and preparation method thereof |
| WO2015133386A1 (en) * | 2014-03-04 | 2015-09-11 | 積水化学工業株式会社 | Adhesive for mounting electronic component and adhesive film for mounting flip chip |
| CN105602494A (en) * | 2016-02-26 | 2016-05-25 | 苏州三和开泰花线织造有限公司 | Organosilicone modified waterborne acrylate electrostatic flocking formaldehyde-free adhesive and preparation method thereof |
| CN106478894A (en) * | 2016-10-03 | 2017-03-08 | 辽宁恒星精细化工有限公司 | High resiliency flocking adhesive |
| CN106590476A (en) * | 2016-11-03 | 2017-04-26 | 东莞市联洲知识产权运营管理有限公司 | Electrostatic flocking adhesive and preparation method thereof |
-
2018
- 2018-09-26 CN CN201811124906.9A patent/CN110951428A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423735A (en) * | 2008-12-05 | 2009-05-06 | 武汉科技学院 | Method for preparing environment-friendly type organosilicon modified acrylic ester binding agent |
| CN102174305A (en) * | 2010-12-14 | 2011-09-07 | 北京高盟新材料股份有限公司 | Acrylate adhesive for reflective cloth and preparation method thereof |
| CN103214993A (en) * | 2013-05-04 | 2013-07-24 | 辽宁恒星精细化工有限公司 | Acrylic ester electrostatic flocking binding agent and preparation method thereof |
| WO2015133386A1 (en) * | 2014-03-04 | 2015-09-11 | 積水化学工業株式会社 | Adhesive for mounting electronic component and adhesive film for mounting flip chip |
| CN104015414A (en) * | 2014-06-18 | 2014-09-03 | 航天海鹰(镇江)特种材料有限公司 | Aerogel composite fabric utilizing aqueous adhesive and preparation method thereof |
| CN105602494A (en) * | 2016-02-26 | 2016-05-25 | 苏州三和开泰花线织造有限公司 | Organosilicone modified waterborne acrylate electrostatic flocking formaldehyde-free adhesive and preparation method thereof |
| CN106478894A (en) * | 2016-10-03 | 2017-03-08 | 辽宁恒星精细化工有限公司 | High resiliency flocking adhesive |
| CN106590476A (en) * | 2016-11-03 | 2017-04-26 | 东莞市联洲知识产权运营管理有限公司 | Electrostatic flocking adhesive and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 李广宇等: "《胶粘与密封技术》", 31 January 2006, 国防工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113637431A (en) * | 2021-08-30 | 2021-11-12 | 惠州市强茂化工科技有限公司 | Pressure-sensitive adhesive, pressure-sensitive adhesive layer, method for preparing pressure-sensitive adhesive and method for preparing pressure-sensitive adhesive layer |
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