CN113429920A - Waterproof and heat-resistant PP hot melt adhesive and preparation method thereof - Google Patents

Waterproof and heat-resistant PP hot melt adhesive and preparation method thereof Download PDF

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Publication number
CN113429920A
CN113429920A CN202110789394.3A CN202110789394A CN113429920A CN 113429920 A CN113429920 A CN 113429920A CN 202110789394 A CN202110789394 A CN 202110789394A CN 113429920 A CN113429920 A CN 113429920A
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Prior art keywords
resistant
hot melt
melt adhesive
heat
modified
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CN202110789394.3A
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Inventor
王海清
吴朋川
赵芬娜
袁少山
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Anhui Guofeng Plastic Industry Co Ltd
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Anhui Guofeng Plastic Industry Co Ltd
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Priority to CN202110789394.3A priority Critical patent/CN113429920A/en
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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
    • C09J151/06—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 homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
    • 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
    • C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
    • C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
    • 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
    • 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
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

Abstract

The invention discloses a waterproof and heat-resistant PP hot melt adhesive and a preparation method thereof, which relate to the technical field of hot melt adhesives and comprise the following components in percentage by mass: 50-55% of organic silicon modified PP, 30-35% of C5 resin, 5-10% of microcrystalline wax, 4-8% of filler and 0.5-2% of plasticizer. According to the invention, the organosilicon modified PP is used as a matrix, so that the water resistance is good, and the components such as C5 resin, microcrystalline wax, filler, plasticizer and the like are added, so that the stability, water resistance and heat resistance of the prepared hot melt adhesive are obviously improved.

Description

Waterproof and heat-resistant PP hot melt adhesive and preparation method thereof
Technical Field
The invention relates to the technical field of hot melt adhesives, in particular to a waterproof and heat-resistant PP hot melt adhesive and a preparation method thereof.
Background
PP has the advantages of no polarity, low viscosity, good stability and water resistance, light color, transparency, low price and the like, and is a good raw material for preparing hot melt adhesives, coatings and building composite materials.
Since PP is a nonpolar molecule, its relative molecular mass is small, structure is irregular, and cohesion is poor, resulting in poor hydrophilicity, antistatic property, mechanical properties, and heat resistance, and the application range is limited.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a waterproof and heat-resistant PP hot melt adhesive and a preparation method thereof, and the stability, the water resistance and the heat resistance of the prepared hot melt adhesive are obviously improved.
The invention provides a waterproof and heat-resistant PP hot melt adhesive which comprises the following components in percentage by mass: 50-55% of organic silicon modified PP, 30-35% of C5 resin, 5-10% of microcrystalline wax, 4-8% of filler and 0.5-2% of plasticizer.
Preferably, the silicone modified PP is prepared as follows: adding PP and xylene into a reaction kettle, stirring and heating until the PP is dissolved, adding dibenzoyl peroxide, slowly adding trienyl triethoxy silane, stirring and reacting, adding acetone after the reaction is finished to obtain a precipitate, filtering the precipitate, and drying in vacuum to constant weight to obtain the organosilicon modified PP.
Preferably, after the addition of the trienyl triethoxy silane is finished, stirring and reacting for 90-120 min at 50-60 ℃; preferably, the vacuum drying temperature is 75-85 ℃.
Preferably, the mass ratio of PP to trienyl triethoxy silane is 2: 7 to 9.
Preferably, the filler is activated calcium carbonate.
Preferably, the plasticizer is dibutyl phthalate.
The invention also provides a preparation method of the waterproof and heat-resistant PP hot melt adhesive, which comprises the steps of adding microcrystalline wax, a filler and a plasticizer into a reaction kettle, and heating to form a melt; and then adding C5 resin and organic silicon modified PP, heating, stirring and mixing, and then cooling at normal temperature to obtain the modified PP.
Preferably, microcrystalline wax, a filler and a plasticizer are added into a reaction kettle and heated to 100-120 ℃ to form a melt; and then adding C5 resin and organic silicon modified PP, heating to 170-180 ℃, stirring and mixing, and then cooling at normal temperature to obtain the modified PP.
Has the advantages that: the modified PP is prepared by adopting trifunctional organosilicon with alkene double bonds to be mixed with PP for grafting reaction under the action of a small amount of peroxide, hydrolyzing silane into silanol under the action of water, and then performing condensation dehydration for crosslinking to finally obtain the organosilicon modified PP. The modified PP is used as a matrix, has good water resistance, and is added with components such as C5 resin, microcrystalline wax, a filler, a plasticizer and the like, so that the stability, the water resistance and the heat resistance of the prepared hot melt adhesive are obviously improved. In addition, the hot melt adhesive has the advantages of easily available raw materials, low cost, simple preparation process and easy control, thereby effectively ensuring the stability of product quality, and the obtained hot melt adhesive has excellent bonding performance, high softening point, convenient storage and convenient popularization and application.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
The formulations of the water and heat resistant PP hotmelt adhesives of examples 1 to 4 are shown in Table 1.
TABLE 1 formulation of water and heat resistant PP Hot melt adhesive in examples 1-4
Figure BDA0003160274510000021
Figure BDA0003160274510000031
The preparation method of the hot melt adhesive comprises the following steps: adding microcrystalline wax, a filler and a plasticizer into a reaction kettle, and heating to 100-120 ℃ to form a melt; and then adding C5 resin and organic silicon modified PP, heating to 170-180 ℃, stirring and mixing, and then cooling at normal temperature to obtain the modified PP.
Comparative example
Compared with example 3, the hot melt adhesive is different from the hot melt adhesive only in that the organosilicon modified PP in example 3 is replaced by unmodified PP in the formula.
The hot melt adhesives prepared in the examples of the invention and comparative examples were tested for their performance.
Melt Flow Rate (MFR)
The test method comprises the following steps: using a melt flow rate tester to test the MFR of a sample, the temperature is 110 ℃, and the load is 2.16 Kg; the results are shown in Table 1.
(II) Peel Strength
The test method comprises the following steps: coating the hot melt adhesive on a base film, and testing the peel strength by using a universal material testing machine according to GB/T2790-1995 standard, wherein the standard of a sample is 80 multiplied by 20 mm; the results are shown in Table 1.
(III) Hot melt adhesive Water resistance stability test
The test method comprises the following steps: soaking the hot melt adhesive in water at 25 ℃ for 8 hours, then airing, and testing MFR and peel strength; the results are shown in Table 2.
(IV) Hot melt adhesive Heat resistance test
The test method comprises the following steps: performing TGA test on the organic silicon modified PP hot melt adhesive and the unmodified PP hot melt adhesive, and testing the thermal decomposition temperatures of the two groups of substances; the results are shown in Table 2.
TABLE 1 Performance parameters of the hotmelt adhesives prepared in examples 1 to 4 and comparative example
Figure BDA0003160274510000041
Table 2 water stability and heat resistance data for hot melt adhesives prepared in example 3 and comparative examples
Figure BDA0003160274510000042
As can be seen from Table 1, the flexibility and the heat adhesion of the heat-seal strength adhesive layer of the hot melt adhesive in the examples of the present invention are significantly improved compared to the comparative examples.
As can be seen from Table 2, the MFR of the two groups of hot melt adhesives is increased, the hot melt adhesives are degraded in the soaking process, the peel strength is reduced, and the MFR of the modified hot melt adhesives in example 3 is smaller than that of the PP hot melt adhesives in the comparative example, which shows that the heat seal strength, the flexibility of the adhesive layer and the heat adhesion of the hot melt adhesives are improved; the modified PP hot melt adhesive has higher peel strength than the PP hot melt adhesive, and the hot melt adhesive prepared from the modified PP has better binding force with a base material; the decomposition temperature of the modified PP hot melt adhesive is higher than that of the PP hot melt adhesive, which shows that the heat resistance of the hot melt adhesive is improved. In conclusion, the stability, heat resistance and water resistance of the modified PP hot melt adhesive are improved.
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 (8)

1. The waterproof and heat-resistant PP hot melt adhesive is characterized by comprising the following components in percentage by mass: 50-55% of organic silicon modified PP, 30-35% of C5 resin, 5-10% of microcrystalline wax, 4-8% of filler and 0.5-2% of plasticizer.
2. The water-resistant and heat-resistant PP hot melt adhesive according to claim 1, wherein the silicone modified PP is prepared by the following steps: adding PP and xylene into a reaction kettle, stirring and heating until the PP is dissolved, adding dibenzoyl peroxide, slowly adding trienyl triethoxy silane, stirring and reacting, adding acetone after the reaction is finished to obtain a precipitate, filtering the precipitate, and drying in vacuum to constant weight to obtain the organosilicon modified PP.
3. The water-resistant heat-resistant PP hot melt adhesive according to claim 2, wherein after the addition of the trienyl triethoxy silane is finished, the mixture is stirred and reacted at 50-60 ℃ for 90-120 min; preferably, the vacuum drying temperature is 75-85 ℃.
4. The water-resistant and heat-resistant PP hot melt adhesive according to claim 2, wherein the mass ratio of PP to the trienyl triethoxy silane is 2: 7 to 9.
5. The water-resistant and heat-resistant PP hot melt adhesive of claim 1, wherein the filler is activated calcium carbonate.
6. The water-resistant and heat-resistant PP hot melt adhesive according to claim 1, wherein the plasticizer is dibutyl phthalate.
7. The preparation method of the water-resistant and heat-resistant PP hot melt adhesive as claimed in any one of claims 1 to 6, wherein microcrystalline wax, a filler and a plasticizer are added into a reaction kettle and heated into a melt; and then adding C5 resin and organic silicon modified PP, heating, stirring and mixing, and then cooling at normal temperature to obtain the modified PP.
8. The preparation method of the water-resistant heat-resistant PP hot melt adhesive according to claim 7, wherein microcrystalline wax, a filler and a plasticizer are added into a reaction kettle and heated to 100-120 ℃ to form a melt; and then adding C5 resin and organic silicon modified PP, heating to 170-180 ℃, stirring and mixing, and then cooling at normal temperature to obtain the modified PP.
CN202110789394.3A 2021-07-13 2021-07-13 Waterproof and heat-resistant PP hot melt adhesive and preparation method thereof Pending CN113429920A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1433451A (en) * 1999-12-22 2003-07-30 埃克森美孚化学专利公司 Adhesive alpha-olefin inter-polymers
US20110060078A1 (en) * 2008-08-15 2011-03-10 Evonik Degussa Gmbh Silane-modified polyolefins having a high degree of functionalization
CN102123860A (en) * 2008-08-15 2011-07-13 赢创德固赛有限责任公司 Use of silane-modified plyolefins as adhesion promoters for the production of flat laminates
CN109486445A (en) * 2017-09-12 2019-03-19 丹阳市丹达防腐设备有限公司 A kind of hot melt adhesive and preparation method thereof for steel lined plastic compound pipeline
CN111363254A (en) * 2020-04-24 2020-07-03 界首市宏利塑料有限公司 High-wear-resistance PP rope

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1433451A (en) * 1999-12-22 2003-07-30 埃克森美孚化学专利公司 Adhesive alpha-olefin inter-polymers
US20110060078A1 (en) * 2008-08-15 2011-03-10 Evonik Degussa Gmbh Silane-modified polyolefins having a high degree of functionalization
CN102123860A (en) * 2008-08-15 2011-07-13 赢创德固赛有限责任公司 Use of silane-modified plyolefins as adhesion promoters for the production of flat laminates
CN109486445A (en) * 2017-09-12 2019-03-19 丹阳市丹达防腐设备有限公司 A kind of hot melt adhesive and preparation method thereof for steel lined plastic compound pipeline
CN111363254A (en) * 2020-04-24 2020-07-03 界首市宏利塑料有限公司 High-wear-resistance PP rope

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