CN113136155A - High-solid-content polyvinyl acetate emulsion adhesive and preparation method thereof - Google Patents
High-solid-content polyvinyl acetate emulsion adhesive and preparation method thereof Download PDFInfo
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- CN113136155A CN113136155A CN202110640911.0A CN202110640911A CN113136155A CN 113136155 A CN113136155 A CN 113136155A CN 202110640911 A CN202110640911 A CN 202110640911A CN 113136155 A CN113136155 A CN 113136155A
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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
- C09J131/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Adhesives based on derivatives of such polymers
- C09J131/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C09J131/04—Homopolymers or copolymers of vinyl acetate
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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
- C09J11/08—Macromolecular additives
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Abstract
The invention discloses a high-solid content polyvinyl acetate emulsion adhesive, which comprises the following raw materials in percentage by mass: 35-45% of water, 50-60% of vinyl acetate, 3-6% of polyvinyl alcohol, 15-20% of trimethyl butanol solvent, 0.5-1% of emulsifier, 1-2% of persulfate, 2-4% of plasticizer, 0.05-0.1% of defoaming agent and 0.05-0.1% of preservative. The invention has reasonable design, high solid content, high bonding strength, environmental protection, no complex process, proper cost, environmental protection and no harmful substances such as aldehydes and the like, and is superior to the market similar vinyl acetate emulsion adhesive.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a high-solid content polyvinyl acetate emulsion adhesive and a preparation method thereof.
Background
The adhesive is organic or inorganic, natural or synthetic substance which can connect the same or more than two homogeneous or heterogeneous products (or materials) together and has enough strength after being cured, at present, the demand of the adhesive in the market is continuously expanded, but the existing adhesive has the defects of general solid content of 50 percent or less, limited bonding strength, containing harmful substances such as o-benzene plasticizer and the like, and therefore, a high-solid content polyvinyl acetate emulsion adhesive and a preparation method thereof are designed to solve the problems.
Disclosure of Invention
The invention aims to solve the existing problems, and provides the high-solid content polyvinyl acetate emulsion adhesive and the preparation method thereof, which have the advantages of high solid content, high bonding strength, environmental protection, no complex process, proper cost, environmental protection and no harmful substances such as aldehydes and the like, and are superior to the similar polyvinyl acetate emulsion adhesive in the market.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-solid content polyvinyl acetate emulsion adhesive comprises the following raw materials in percentage by mass: 35-45% of water, 50-60% of vinyl acetate, 3-6% of polyvinyl alcohol, 15-20% of trimethyl butanol solvent, 0.5-1% of emulsifier, 1-2% of persulfate, 2-4% of plasticizer, 0.05-0.1% of defoaming agent and 0.05-0.1% of preservative.
A preparation method of a high-solid content polyvinyl acetate emulsion adhesive comprises the following steps:
s1: preparing the following raw materials in percentage by mass: 35-45% of water, 50-60% of vinyl acetate, 3-6% of polyvinyl alcohol, 15-20% of trimethyl butanol solvent, 0.5-1% of emulsifier, 1-2% of persulfate, 2-4% of plasticizer, 0.05-0.1% of defoaming agent and 0.05-0.1% of preservative;
s2: dividing water into a first part of water and a second part of water according to a ratio of 4:6, preparing a stirring reaction kettle, cleaning the interior of the stirring reaction kettle, sequentially putting the first part of water and polyvinyl alcohol into the stirring reaction kettle after cleaning, starting the stirring reaction kettle, regulating the temperature of the stirring reaction kettle to 90 ℃, starting a stirring shaft of the stirring reaction kettle, mixing and stirring, wherein the rotating speed of the stirring shaft is 800 plus 1200 rpm, the mixing and stirring time is 10-15min, closing the stirring shaft after stirring, and performing heat preservation reaction for 2-2.5 h;
s3: preparing a first reaction cup, sequentially putting a second part of water and persulfate into the first reaction cup, preparing a stirring rod, carrying out mixed dissolution work on the interior of the first reaction cup through the stirring rod, wherein the mixed dissolution work time is 10-15min to obtain persulfate solution, and dividing the persulfate solution into a first part of persulfate solution and a second part of persulfate solution according to the ratio of 1: 1;
s4: putting the trimethyl butanol solvent into a stirring reaction kettle, adjusting the rotation speed of a stirring shaft to 800 plus materials at 1000 rpm, and stirring for 5-10 min;
s5: adjusting the temperature of the stirring reaction kettle to 75-80 ℃, heating for 2-3min, adding the emulsifier into the stirring reaction kettle, and continuing to perform heat preservation for 20-25 min; dividing vinyl acetate into a first part of vinyl acetate and a second part of vinyl acetate according to the ratio of 1:7, sequentially putting the first part of persulfate solution and the first part of vinyl acetate into a stirring reaction kettle, and then continuing to perform heat preservation for 3.5-4 hours; sequentially putting a second part of persulfate solution and a second part of vinyl acetate into a stirring reaction kettle, starting a stirring shaft, carrying out mixing and stirring work for 30-35min, carrying out vacuum extraction work after the mixing and stirring work is finished to obtain a mixed solution, and putting the mixed solution into a second reaction cup;
s6: cooling the mixed solution to 45-50 ℃, and then injecting a plasticizer; after the injection is finished, continuing cooling to 37-40 ℃, and then injecting a defoaming agent and a preservative;
s7: and (3) carrying out mixing and stirring work on the interior of the second reaction cup through a stirring rod, wherein the mixing and stirring time is 20-25min, after the mixing and stirring are finished, carrying out filtering work on the interior of the second reaction cup through a filter screen, and after the filtering is finished, obtaining the high-solid content polyvinyl acetate emulsion adhesive.
Preferably, in S7, the number of times of filtering by the filter screen is 3-6.
Compared with the prior art, the invention has the beneficial effects that:
the invention has reasonable design, high solid content, high bonding strength, environmental protection, no complex process, proper cost, environmental protection and no harmful substances such as aldehydes and the like, and is superior to the market similar vinyl acetate emulsion adhesive.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
A high-solid content polyvinyl acetate emulsion adhesive comprises the following raw materials in percentage by mass: 35-45% of water, 50-60% of vinyl acetate, 3-6% of polyvinyl alcohol, 15-20% of trimethyl butanol solvent, 0.5-1% of emulsifier, 1-2% of persulfate, 2-4% of plasticizer, 0.05-0.1% of defoaming agent and 0.05-0.1% of preservative.
Example 1
A preparation method of a high-solid content polyvinyl acetate emulsion adhesive comprises the following steps:
s1: preparing the following raw materials in percentage by mass: 35% of water, 50% of vinyl acetate, 3% of polyvinyl alcohol, 15% of trimethyl butanol solvent, 0.5% of emulsifier, 1% of persulfate, 2% of plasticizer, 0.05% of defoaming agent and 0.05% of preservative;
s2: dividing water into a first part of water and a second part of water according to a ratio of 4:6, preparing a stirring reaction kettle, cleaning the interior of the stirring reaction kettle, sequentially putting the first part of water and polyvinyl alcohol into the stirring reaction kettle after cleaning, starting the stirring reaction kettle, regulating the temperature of the stirring reaction kettle to 90 ℃, starting a stirring shaft of the stirring reaction kettle, mixing and stirring, wherein the rotating speed of the stirring shaft is 800 revolutions per minute, the mixing and stirring time is 10 minutes, closing the stirring shaft after stirring, and performing heat preservation reaction for 2 hours;
s3: preparing a first reaction cup, sequentially putting a second part of water and persulfate into the first reaction cup, preparing a stirring rod, carrying out mixed dissolution work on the interior of the first reaction cup through the stirring rod, wherein the mixed dissolution work time is 10min, so as to obtain persulfate solution, and dividing the persulfate solution into a first part of persulfate solution and a second part of persulfate solution according to the ratio of 1: 1;
s4: putting a trimethyl butanol solvent into a stirring reaction kettle, adjusting the rotation speed of a stirring shaft to 800 revolutions per minute, and stirring for 50 minutes;
s5: adjusting the temperature of the stirring reaction kettle to 75 ℃, heating for 2min, putting the emulsifier into the stirring reaction kettle, and continuing to perform heat preservation for 20 min; dividing vinyl acetate into a first part of vinyl acetate and a second part of vinyl acetate according to the ratio of 1:7, sequentially putting the first part of persulfate solution and the first part of vinyl acetate into a stirring reaction kettle, and then continuing to perform heat preservation for 3.5 hours; sequentially putting a second part of persulfate solution and a second part of vinyl acetate into a stirring reaction kettle, starting a stirring shaft, carrying out mixing and stirring work for 30min, carrying out vacuum extraction work after the mixing and stirring work is finished to obtain a mixed solution, and putting the mixed solution into a second reaction cup;
s6: cooling the mixed solution to 45 ℃, and then injecting a plasticizer; after the injection is finished, continuing cooling to 37 ℃, and then injecting a defoaming agent and a preservative;
s7: and (3) mixing and stirring the interior of the second reaction cup by using a stirring rod for 20min, filtering the interior of the second reaction cup by using a filter screen after the mixing and stirring are finished, wherein the filter screen is used for filtering for 3 times, and after the filtering is finished, the high-solid-content polyvinyl acetate emulsion adhesive can be obtained.
Example 2
A preparation method of a high-solid content polyvinyl acetate emulsion adhesive comprises the following steps:
s1: preparing the following raw materials in percentage by mass: 37% of water, 54% of vinyl acetate, 4% of polyvinyl alcohol, 17% of trimethyl butanol solvent, 0.7% of emulsifier, 1.2% of persulfate, 2.5% of plasticizer, 0.07% of defoaming agent and 0.07% of preservative;
s2: dividing water into a first part of water and a second part of water according to a ratio of 4:6, preparing a stirring reaction kettle, cleaning the interior of the stirring reaction kettle, sequentially putting the first part of water and polyvinyl alcohol into the stirring reaction kettle after cleaning is finished, starting the stirring reaction kettle, regulating the temperature of the stirring reaction kettle to 90 ℃, starting a stirring shaft of the stirring reaction kettle, mixing and stirring materials, wherein the rotating speed of the stirring shaft is 900 revolutions per minute, the mixing and stirring time is 12 minutes, closing the stirring shaft after stirring is finished, and carrying out heat preservation reaction for 2.2 hours;
s3: preparing a first reaction cup, sequentially putting a second part of water and persulfate into the first reaction cup, preparing a stirring rod, carrying out mixed dissolution work on the interior of the first reaction cup through the stirring rod, wherein the mixed dissolution work time is 12min, so as to obtain persulfate solution, and dividing the persulfate solution into a first part of persulfate solution and a second part of persulfate solution according to the ratio of 1: 1;
s4: putting a trimethyl butanol solvent into a stirring reaction kettle, adjusting the rotation speed of a stirring shaft to 850 revolutions per minute, and stirring for 7 minutes;
s5: adjusting the temperature of the stirring reaction kettle to 77 ℃, heating for 2.2min, adding the emulsifier into the stirring reaction kettle, and continuing to perform heat preservation for 22 min; dividing vinyl acetate into a first part of vinyl acetate and a second part of vinyl acetate according to the ratio of 1:7, sequentially putting the first part of persulfate solution and the first part of vinyl acetate into a stirring reaction kettle, and then continuing to perform heat preservation for 3.7 hours; sequentially putting a second part of persulfate solution and a second part of vinyl acetate into a stirring reaction kettle, starting a stirring shaft, carrying out mixing and stirring work for 32min, carrying out vacuum extraction work after the mixing and stirring work is finished to obtain a mixed solution, and putting the mixed solution into a second reaction cup;
s6: cooling the mixed solution to 47 ℃, and then injecting a plasticizer; after the injection is finished, continuing cooling to 38 ℃, and then injecting a defoaming agent and a preservative;
s7: and (3) mixing and stirring the interior of the second reaction cup by using a stirring rod for 22min, filtering the interior of the second reaction cup by using a filter screen after the mixing and stirring are finished, wherein the filter screen is used for filtering for 4 times, and after the filtering is finished, the high-solid-content polyvinyl acetate emulsion adhesive can be obtained.
Example 3
A preparation method of a high-solid content polyvinyl acetate emulsion adhesive comprises the following steps:
s1: preparing the following raw materials in percentage by mass: 42% of water, 58% of vinyl acetate, 5% of polyvinyl alcohol, 18% of trimethyl butanol solvent, 0.9% of emulsifier, 1.8% of persulfate, 3.5% of plasticizer, 0.09% of defoaming agent and 0.09% of preservative;
s2: dividing water into a first part of water and a second part of water according to a ratio of 4:6, preparing a stirring reaction kettle, cleaning the interior of the stirring reaction kettle, sequentially putting the first part of water and polyvinyl alcohol into the stirring reaction kettle after cleaning is finished, starting the stirring reaction kettle, regulating the temperature of the stirring reaction kettle to 90 ℃, starting a stirring shaft of the stirring reaction kettle, mixing and stirring materials, wherein the rotating speed of the stirring shaft is 1100 r/min, the mixing and stirring time is 14min, closing the stirring shaft after stirring is finished, and carrying out heat preservation reaction for 2.4 h;
s3: preparing a first reaction cup, sequentially putting a second part of water and persulfate into the first reaction cup, preparing a stirring rod, carrying out mixed dissolution work on the interior of the first reaction cup through the stirring rod, wherein the mixed dissolution work time is 14min, so as to obtain persulfate solution, and dividing the persulfate solution into a first part of persulfate solution and a second part of persulfate solution according to the ratio of 1: 1;
s4: putting a trimethyl butanol solvent into a stirring reaction kettle, adjusting the rotation speed of a stirring shaft to 950 revolutions per minute, and stirring for 9 minutes;
s5: adjusting the temperature of the stirring reaction kettle to 79 ℃, heating for 2.8min, putting the emulsifier into the stirring reaction kettle, and continuing to perform heat preservation for 24 min; dividing vinyl acetate into a first part of vinyl acetate and a second part of vinyl acetate according to the ratio of 1:7, sequentially putting the first part of persulfate solution and the first part of vinyl acetate into a stirring reaction kettle, and then continuing to perform heat preservation for 3.9 hours; sequentially putting a second part of persulfate solution and a second part of vinyl acetate into a stirring reaction kettle, starting a stirring shaft, carrying out mixing and stirring work for 34min, carrying out vacuum extraction work after the mixing and stirring work is finished to obtain a mixed solution, and putting the mixed solution into a second reaction cup;
s6: cooling the mixed solution to 49 ℃, and then injecting a plasticizer; after the injection is finished, continuing cooling to 39 ℃, and then injecting a defoaming agent and a preservative;
s7: and (3) mixing and stirring the interior of the second reaction cup by using a stirring rod for 24min, filtering the interior of the second reaction cup by using a filter screen after the mixing and stirring are finished, wherein the filter screen is used for filtering for 5 times, and after the filtering is finished, the high-solid-content polyvinyl acetate emulsion adhesive can be obtained.
Example 4
A preparation method of a high-solid content polyvinyl acetate emulsion adhesive comprises the following steps:
s1: preparing the following raw materials in percentage by mass: 45% of water, 60% of vinyl acetate, 6% of polyvinyl alcohol, 20% of a trimethyl butanol solvent, 1% of an emulsifier, 2% of persulfate, 4% of a plasticizer, 0.1% of a defoaming agent and 0.1% of a preservative;
s2: dividing water into a first part of water and a second part of water according to a ratio of 4:6, preparing a stirring reaction kettle, cleaning the interior of the stirring reaction kettle, sequentially putting the first part of water and polyvinyl alcohol into the stirring reaction kettle after cleaning is finished, starting the stirring reaction kettle, regulating the temperature of the stirring reaction kettle to 90 ℃, starting a stirring shaft of the stirring reaction kettle, mixing and stirring materials, wherein the rotating speed of the stirring shaft is 1200 revolutions per minute, the mixing and stirring time is 15 minutes, closing the stirring shaft after stirring is finished, and carrying out heat preservation reaction for 2.5 hours;
s3: preparing a first reaction cup, sequentially putting a second part of water and persulfate into the first reaction cup, preparing a stirring rod, carrying out mixed dissolution work on the interior of the first reaction cup through the stirring rod, wherein the mixed dissolution work time is 15min to obtain persulfate solution, and dividing the persulfate solution into a first part of persulfate solution and a second part of persulfate solution according to the ratio of 1: 1;
s4: putting a trimethyl butanol solvent into a stirring reaction kettle, adjusting the rotation speed of a stirring shaft to 1000 revolutions per minute, and stirring for 10 minutes;
s5: adjusting the temperature of the stirring reaction kettle to 80 ℃, heating for 3min, putting the emulsifier into the stirring reaction kettle, and continuing to perform heat preservation for 25 min; dividing vinyl acetate into a first part of vinyl acetate and a second part of vinyl acetate according to the ratio of 1:7, sequentially putting the first part of persulfate solution and the first part of vinyl acetate into a stirring reaction kettle, and then continuing to perform heat preservation for 4 hours; sequentially putting a second part of persulfate solution and a second part of vinyl acetate into a stirring reaction kettle, starting a stirring shaft, carrying out mixing and stirring work for 35min, carrying out vacuum extraction work after the mixing and stirring work is finished to obtain a mixed solution, and putting the mixed solution into a second reaction cup;
s6: cooling the mixed solution to 50 ℃, and then injecting a plasticizer; after the injection is finished, continuing cooling to 40 ℃, and then injecting a defoaming agent and a preservative;
s7: and (3) mixing and stirring the interior of the second reaction cup by using a stirring rod for 25min, filtering the interior of the second reaction cup by using a filter screen after the mixing and stirring are finished, wherein the filter screen is used for filtering for 6 times, and after the filtering is finished, the high-solid-content polyvinyl acetate emulsion adhesive can be obtained.
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 person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (3)
1. The high-solid content polyvinyl acetate emulsion adhesive is characterized by comprising the following raw materials in percentage by mass: 35-45% of water, 50-60% of vinyl acetate, 3-6% of polyvinyl alcohol, 15-20% of trimethyl butanol solvent, 0.5-1% of emulsifier, 1-2% of persulfate, 2-4% of plasticizer, 0.05-0.1% of defoaming agent and 0.05-0.1% of preservative.
2. The method for preparing high-solid content polyvinyl acetate emulsion adhesive according to claim 1, which is characterized by comprising the following steps:
s1: preparing the following raw materials in percentage by mass: 35-45% of water, 50-60% of vinyl acetate, 3-6% of polyvinyl alcohol, 15-20% of trimethyl butanol solvent, 0.5-1% of emulsifier, 1-2% of persulfate, 2-4% of plasticizer, 0.05-0.1% of defoaming agent and 0.05-0.1% of preservative;
s2: dividing water into a first part of water and a second part of water according to a ratio of 4:6, preparing a stirring reaction kettle, cleaning the interior of the stirring reaction kettle, sequentially putting the first part of water and polyvinyl alcohol into the stirring reaction kettle after cleaning, starting the stirring reaction kettle, regulating the temperature of the stirring reaction kettle to 90 ℃, starting a stirring shaft of the stirring reaction kettle, mixing and stirring, wherein the rotating speed of the stirring shaft is 800 plus 1200 rpm, the mixing and stirring time is 10-15min, closing the stirring shaft after stirring, and performing heat preservation reaction for 2-2.5 h;
s3: preparing a first reaction cup, sequentially putting a second part of water and persulfate into the first reaction cup, preparing a stirring rod, carrying out mixed dissolution work on the interior of the first reaction cup through the stirring rod, wherein the mixed dissolution work time is 10-15min to obtain persulfate solution, and dividing the persulfate solution into a first part of persulfate solution and a second part of persulfate solution according to the ratio of 1: 1;
s4: putting the trimethyl butanol solvent into a stirring reaction kettle, adjusting the rotation speed of a stirring shaft to 800 plus materials at 1000 rpm, and stirring for 5-10 min;
s5: adjusting the temperature of the stirring reaction kettle to 75-80 ℃, heating for 2-3min, adding the emulsifier into the stirring reaction kettle, and continuing to perform heat preservation for 20-25 min; dividing vinyl acetate into a first part of vinyl acetate and a second part of vinyl acetate according to the ratio of 1:7, sequentially putting the first part of persulfate solution and the first part of vinyl acetate into a stirring reaction kettle, and then continuing to perform heat preservation for 3.5-4 hours; sequentially putting a second part of persulfate solution and a second part of vinyl acetate into a stirring reaction kettle, starting a stirring shaft, carrying out mixing and stirring work for 30-35min, carrying out vacuum extraction work after the mixing and stirring work is finished to obtain a mixed solution, and putting the mixed solution into a second reaction cup;
s6: cooling the mixed solution to 45-50 ℃, and then injecting a plasticizer; after the injection is finished, continuing cooling to 37-40 ℃, and then injecting a defoaming agent and a preservative;
s7: and (3) carrying out mixing and stirring work on the interior of the second reaction cup through a stirring rod, wherein the mixing and stirring time is 20-25min, after the mixing and stirring are finished, carrying out filtering work on the interior of the second reaction cup through a filter screen, and after the filtering is finished, obtaining the high-solid content polyvinyl acetate emulsion adhesive.
3. The high-solid content polyvinyl acetate emulsion adhesive and the preparation method thereof according to claim 2, wherein in S7, the filter screen filtering times are 3-6.
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| CN202110640911.0A CN113136155A (en) | 2021-06-09 | 2021-06-09 | High-solid-content polyvinyl acetate emulsion adhesive and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114437652A (en) * | 2022-03-01 | 2022-05-06 | 沈阳爱克浩博化工有限公司 | Special modified polyvinyl acetate emulsion adhesive and preparation method thereof |
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| JP2005187704A (en) * | 2003-12-26 | 2005-07-14 | Konishi Co Ltd | High-speed adhesive composition |
| CN105131866A (en) * | 2015-09-23 | 2015-12-09 | 台州市顶立胶粘剂有限公司 | Water-based adhesive for iron-sheet panel composite veneer and preparation method thereof |
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| CN1498936A (en) * | 2002-11-06 | 2004-05-26 | 中国科学院成都有机化学研究所 | Method for synthesizing and preparing avirulent adhesion agent |
| JP2005187704A (en) * | 2003-12-26 | 2005-07-14 | Konishi Co Ltd | High-speed adhesive composition |
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