CN110527307A - A kind of high-polymer strong intersects film reaction type adhesive waterproof coil and preparation method thereof - Google Patents

A kind of high-polymer strong intersects film reaction type adhesive waterproof coil and preparation method thereof Download PDF

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Publication number
CN110527307A
CN110527307A CN201810501539.3A CN201810501539A CN110527307A CN 110527307 A CN110527307 A CN 110527307A CN 201810501539 A CN201810501539 A CN 201810501539A CN 110527307 A CN110527307 A CN 110527307A
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CN
China
Prior art keywords
reaction type
type adhesive
film reaction
parts
adhesive waterproof
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Withdrawn
Application number
CN201810501539.3A
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Chinese (zh)
Inventor
郑建林
郑伟
郑娜
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Weifang Xing Wang Waterproofing Material Co Ltd
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Weifang Xing Wang Waterproofing Material Co Ltd
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Priority to CN201810501539.3A priority Critical patent/CN110527307A/en
Publication of CN110527307A publication Critical patent/CN110527307A/en
Withdrawn legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The present invention provides the preparation method that a kind of high-polymer strong intersects film reaction type adhesive waterproof coil, the preparation including surface layer waterproof layer, including be first ultrasonically treated, repressurization to 4kgf/cm2, and keep 25min, it is 1-3 seconds last in so that pressure is down to O;The raw material of waterproof roll includes modified pitch, butadiene-styrene rubber, vinyl pyrrolidone-vinyl acetate copolymer, polyethylene glycol oxide, polyvinyl alcohol, cellulose acetate, C_4 hydrocarbon, tackifier, methyl acrylate, softening agent, different tridecyl alcohol phosphate ester and diisooctyl phthalate;High-polymer strong of the invention intersects film reaction type adhesive waterproof coil, peel strength is 3.7N/mm, wear-resistant power reaches 10028rad, while having effect outstanding to fire-retardant, has in anti-skidding, wear-resisting, flame-retardancy requirements waterproofing works especially suitable for all kinds of industrial and mining enterprises, parking lot, sports ground etc..

Description

A kind of high-polymer strong intersects film reaction type adhesive waterproof coil and preparation method thereof
Technical field
The invention belongs to waterproof roll technical fields, are related to a kind of high-polymer strong intersection film reaction type self-adhesion waterproof roll Material, and in particular to a kind of high-polymer strong intersects film reaction type adhesive waterproof coil and preparation method thereof.
Background technique
Waterproof roll is the waterproof material of a kind of great development prospect and application prospect, have low temperature flexibility, self-healing property and The good feature of adhesive property, can room temperature construction, speed of application is fast, meets environmental requirement.
Currently, existing high-polymer strong intersects film reaction type adhesive waterproof coil waterproof roll in the prior art anti- It is aqueous can on continue to optimize, but still have the defects that comprehensive performance cannot be improved simultaneously, this defect is in certain journey The application range and development of product are constrained on degree.
In conclusion how to advanced optimize the comprehensive performance of waterproof roll, it is urgently to be resolved to become those skilled in the art The technical issues of.
Summary of the invention
Against the above deficiency, technical problem to be solved by the invention is to provide a kind of high-polymer strongs to intersect film by the present invention Response type adhesive waterproof coil and preparation method thereof.Following goal of the invention may be implemented in the present invention:
High-polymer strong of the invention intersects film reaction type adhesive waterproof coil, has peel strength height, pitch fracture elongation The features such as small, waterproof performances and heat aging are good, wear-resistant power is strong, is slided in high, 70 DEG C of heat resistances detections, at the same to it is fire-retardant have it is prominent Effect out has anti-skidding, wear-resisting, flame-retardancy requirements waterproofing works especially suitable for all kinds of industrial and mining enterprises, parking lot, sports ground etc. In.
In order to solve the above technical problems, using following technical scheme:
A kind of high-polymer strong intersects the preparation method of film reaction type adhesive waterproof coil, which is characterized in that the method, including The preparation of surface layer waterproof layer.
As currently preferred technical solution, the preparation of the surface layer waterproof layer includes the following steps:
(1) each raw material is weighed by formula;
(2) according to the ratio by modified pitch, softening agent, vinyl pyrrolidone-vinyl acetate copolymer, methyl acrylate, polyoxy Change ethylene, polyvinyl alcohol and diisooctyl phthalate and be warming up to 175 DEG C, open stirring, adds under 120rad/min rate Enter C_4 hydrocarbon, is ultrasonically treated 30min;
(3) it is forced into 4kgf/cm2, and 25min is kept, so that pressure is down to Okgf/cm in 1-3 seconds2
(4) half of different tridecyl alcohol phosphate ester quality is added, 50min is stirred at 155 DEG C, is ultrasonically treated 30min, temperature 67 DEG C, power 345W;
(5) remaining different tridecyl alcohol phosphate ester is added, is stirred 1 hour after adding;
It is cooling, 35min is kept the temperature under the conditions of 75 DEG C.
As currently preferred technical solution, in the step (2), the process conditions of ultrasonic treatment are as follows: ultrasonic temperature 66 DEG C of degree, power 355W.
A kind of high-polymer strong intersection film reaction type adhesive waterproof coil, which is characterized in that by surface layer waterproof layer, self-adhesive layer It is formed with PET film layer, wherein waterproof layer raw material in surface layer includes modified pitch and butadiene-styrene rubber.
As currently preferred technical solution, the raw material includes: modified pitch, butadiene-styrene rubber, ethenyl pyrrolidone It is ketone-vinyl acetate copolymer, polyethylene glycol oxide, polyvinyl alcohol, cellulose acetate, C_4 hydrocarbon, tackifier, methyl acrylate, soft Agent, different tridecyl alcohol phosphate ester and diisooctyl phthalate.
As currently preferred technical solution, the raw material includes: 35 parts of modified pitch, butadiene-styrene rubber by weight 18 parts, 18 parts of vinyl pyrrolidone-vinyl acetate copolymer, 6 parts of polyethylene glycol oxide, 3 parts of polyvinyl alcohol, cellulose acetate 12 Part, 0.5 part of C_4 hydrocarbon, 6 parts of tackifier, 4 parts of methyl acrylate, 5 parts of softening agent, 5 parts of different tridecyl alcohol phosphate ester and O-phthalic 8 parts of sour diisodecyl ester.
As currently preferred technical solution, the tackifier, by pitch tackifier GXJ- I and terpene resin T-110 Composition, GXJ- I and terpene resin T-110 mass ratio are 3:7.
As currently preferred technical solution, the different tridecyl alcohol phosphate ester, pH value 3.3-4.1, solid content 96.5- 99.5%。
As currently preferred technical solution, the C_4 hydrocarbon, mono-olefin content accounting is 2.2-10.6%, alkadienes Content accounting is 6.8-22.9%, and methyl tertbutyl ether content is 1.5-12.4%, and sulfur content is lower than 5ppm.
As currently preferred technical solution, the high-polymer strong intersects film reaction type adhesive waterproof coil, material with Peel strength between coiled material is 3.1N/mm, and the peel strength between coiled material and aluminium is 3.7N/mm, and wear-resistant power reaches 10028rad。
The invention adopts the above technical scheme, compared with prior art, has the advantage that
High-polymer strong of the invention possesses following benefit performance while intersecting film reaction type adhesive waterproof coil:
(1) high-polymer strong of the invention intersects film reaction type adhesive waterproof coil, and peel strength is high, between coiled material and coiled material Peel strength is 3.1N/mm, and the peel strength between coiled material and aluminium is 3.7N/mm;
(2) pitch fracture elongation is up to 264%;
(3) 70 DEG C of heat resistance detection slidings are 0.5mm;
(4) low temperature flexibility is -35 DEG C without fracture;
(5) impermeability, 0.5MPa180min are waterproof;
(6) heat aging is good, and pulling force conservation rate is 95%, and elongation percentage is 312% when maximum pull, -32 DEG C of low temperature flexibility without fracture, Peel strength between coiled material and aluminium sheet is 2.9N/mm;
(7) waterproof layer wear-resistant power in surface layer is strong, is resistant to 10028rad;
(8) good flame resistance, total burning time are 11.1s.
Specific embodiment
A kind of high-polymer strong of embodiment 1 intersects film reaction type adhesive waterproof coil
A kind of high-polymer strong of the invention intersects film reaction type adhesive waterproof coil, including following raw material: modified pitch, butylbenzene Rubber, vinyl pyrrolidone-vinyl acetate copolymer, polyethylene glycol oxide, polyvinyl alcohol, cellulose acetate, C_4 hydrocarbon, thickening Agent, methyl acrylate, softening agent, different tridecyl alcohol phosphate ester and diisooctyl phthalate;
The raw material includes: that 35 parts of modified pitch, 18 parts of butadiene-styrene rubber, vinyl pyrrolidone-vinyl acetate are total by weight 18 parts of aggressiveness, 6 parts of polyethylene glycol oxide, 3 parts of polyvinyl alcohol, 12 parts of cellulose acetate, 0.5 part of C_4 hydrocarbon, 6 parts of tackifier, propylene 4 parts of sour methyl esters, 5 parts of softening agent, 5 parts of different tridecyl alcohol phosphate ester and 8 parts of diisooctyl phthalate;
The tackifier are made of pitch tackifier GXJ- I and terpene resin T-110, GXJ- I and terpene resin T-110 mass Than for 3:7;
The pitch tackifier GXJ- I is purchased from Jinan Zi An Chemical Co., Ltd.;
The terpene resin T-110 connects Industrial Co., Ltd. purchased from Shanghai three;
The different tridecyl alcohol phosphate ester, pH value 3.3-4.1, solid content 96.5-99.5%;
The C_4 hydrocarbon, mono-olefin content accounting are 2.2-10.6%, and diene content accounting is 6.8-22.9%, methyl tertbutyl Ether content is 1.5-12.4%, and sulfur content is lower than 5ppm;
The softening agent, dynamic viscosity is 30-40 at 15.6 DEG C 0.98,100 DEG C of lower density >, and 230 DEG C of flash-point >, acid value is 0.08, coloration > 4.5, volatile matter 0.92%, ductility 100cm;
The diisooctyl phthalate, 20 DEG C of viscosity 128-136mPa.s, volume resistivity 4.2 × 109Ω .m, 20 DEG C close Spend 0.965-0.967g/cm3
Comparative example 1- comparative example 4: on that basis of example 1, only change the weight of tackifier, different tridecyl alcohol phosphate ester and C_4 hydrocarbon Part, change as shown in table 1:
Table 1:
A kind of high-polymer strong of embodiment 2 intersects the preparation method of film reaction type adhesive waterproof coil, and high-polymer strong intersects film Response type adhesive waterproof coil includes surface layer waterproof layer, self-adhesive layer and PET film layer, wherein the preparation method of surface layer waterproof layer, such as Lower step:
(1) quality is weighed by formula described in embodiment, it is spare;
(2) according to the ratio by modified pitch, softening agent, vinyl pyrrolidone-vinyl acetate copolymer, methyl acrylate, polyoxy Change ethylene, polyvinyl alcohol and diisooctyl phthalate and put into reaction kettle, be warming up to 175 DEG C, opens stirring, In C_4 hydrocarbon is added under 120rad/min rate, is ultrasonically treated 30min;
The process conditions of ultrasonic treatment are as follows: 66 DEG C of ultrasonication temperature, power 355W;
(3) mixture that step (2) obtains is put into pressure pan, when so that temperature is raised to 180 DEG C with heat-conducting oil heating, fourth is added Benzene rubber, cellulose acetate and tackifier, stir evenly, and are forced into 4kgf/cm2, and 25min is kept, keep its pressure uniform, so Pressure is set to be down to Okgf/cm suddenly in 1-3 seconds afterwards2
(4) mixture that step (3) obtain is added to the half of different tridecyl alcohol phosphate ester quality, stirs 50min at 155 DEG C, Be ultrasonically treated 30min, 67 DEG C of temperature, power 345W;
(5) remaining different tridecyl alcohol phosphate ester is added, is stirred 1 hour after adding;
(6) cooling, 35min is kept the temperature under the conditions of 75 DEG C, after continuing cool to room temperature, quality inspection obtains surface layer waterproof layer;
(7) surface layer waterproof layer is compound by hot pressing with other two layers, it is anti-to obtain a kind of high-polymer strong intersection film of the invention Answer type adhesive waterproof coil.
A kind of high-polymer strong of the invention intersects the effectiveness indicator of film reaction type adhesive waterproof coil, such as the following table 1 institute Show:
Wherein, in table data corresponding to embodiment 1 and comparative example 1-4 by the formula of embodiment 1 and comparative example 1-4 according to reality Preparation method described in example 2 is applied to be prepared.
Table 1: effectiveness indicator
Remarks: the processing that heat aging uses are as follows: 70 DEG C, 168h;The index of variation without exception in thermal stability has: nothing rises Drum, fold, sliding, trickling;Total burning time uses UL94.
From the above data:
(1) properties that the high-polymer strong of the embodiment of the present invention 1 intersects film reaction type adhesive waterproof coil all obtain simultaneously Biggish raising:
(1) high-polymer strong of the invention intersects film reaction type adhesive waterproof coil, and peel strength is high, between coiled material and coiled material Peel strength is 3.1N/mm, and the peel strength between coiled material and aluminium is 3.7N/mm;
(2) pitch fracture elongation is up to 264%;
(3) 70 DEG C of heat resistance detection slidings are 0.5mm;
(4) low temperature flexibility is -35 DEG C without fracture;
(5) impermeability, 0.5MPa180min are waterproof;
(6) heat aging is good, and pulling force conservation rate is 95%, and elongation percentage is 312% when maximum pull, -32 DEG C of low temperature flexibility without fracture, Peel strength between coiled material and aluminium sheet is 2.9N/mm;
(7) waterproof layer wear-resistant power in surface layer is strong, is resistant to 10028rad;
(8) good flame resistance, total burning time are 11.1s.
(2) by embodiment 1 and comparative example 1-3 it is found that high-polymer strong of the invention intersects film reaction type self-adhesion waterproof roll Material, peel strength, pitch fracture elongation, heat resistance, low temperature flexibility, impermeability, heat aging, waterproof layer is wear-resistant power are all It improves a lot, using the formula containing tackifier, different tridecyl alcohol phosphate ester and C_4 hydrocarbon, using ultrasonic treatment and high pressure rapid drawdown Method promote reaction process and the mixed uniformity to improve the compatibility between each formula, obtained function admirable Waterproof roll.
(3) by embodiment 1 and comparative example 4 it is found that high-polymer strong of the invention intersects film reaction type self-adhesion waterproof roll Material, although the adhesive waterproof coil of comparative example 4 is not much different compared with Example 1 in flame retardant property, peel strength, Pitch fracture elongation, heat aging and wear-resistant power etc. are far away from the embodiment of the present invention 1.
Unless otherwise indicated, percentage of the present invention is weight percent, and ratio of the present invention is Mass ratio.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention, All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention Within protection scope.

Claims (10)

1. the preparation method that a kind of high-polymer strong intersects film reaction type adhesive waterproof coil, which is characterized in that the method, packet Include the preparation of surface layer waterproof layer.
2. a kind of high-polymer strong according to claim 1 intersects the preparation method of film reaction type adhesive waterproof coil, It is characterized in that, the preparation of the surface layer waterproof layer includes the following steps:
(1) each raw material is weighed by formula;
(2) according to the ratio by modified pitch, softening agent, vinyl pyrrolidone-vinyl acetate copolymer, methyl acrylate, polyoxy Change ethylene, polyvinyl alcohol and diisooctyl phthalate and be warming up to 175 DEG C, open stirring, adds under 120rad/min rate Enter C_4 hydrocarbon, is ultrasonically treated 30min;
(3) it is forced into 4kgf/cm2, and 25min is kept, so that pressure is down to Okgf/cm in 1-3 seconds2
(4) half of different tridecyl alcohol phosphate ester quality is added, 50min is stirred at 155 DEG C, is ultrasonically treated 30min, temperature 67 DEG C, power 345W;
(5) remaining different tridecyl alcohol phosphate ester is added, is stirred 1 hour after adding;
(6) cooling, 35min is kept the temperature under the conditions of 75 DEG C.
3. a kind of high-polymer strong according to claim 1 intersects the preparation method of film reaction type adhesive waterproof coil, It is characterized in that, in the step (2), the process conditions of ultrasonic treatment are as follows: ultrasound uses 66 DEG C of temperature, power 355W.
4. a kind of high-polymer strong intersects film reaction type adhesive waterproof coil, which is characterized in that by surface layer waterproof layer, self-adhesive layer and PET film layer composition, wherein waterproof layer raw material in surface layer includes modified pitch and butadiene-styrene rubber.
5. a kind of high-polymer strong according to claim 3 intersects film reaction type adhesive waterproof coil, which is characterized in that institute Stating raw material includes: modified pitch, butadiene-styrene rubber, vinyl pyrrolidone-vinyl acetate copolymer, polyethylene glycol oxide, polyethylene Alcohol, cellulose acetate, C_4 hydrocarbon, tackifier, methyl acrylate, softening agent, different tridecyl alcohol phosphate ester and phthalic acid two are different Last of the ten Heavenly stems ester.
6. a kind of high-polymer strong according to claim 4 intersects film reaction type adhesive waterproof coil, which is characterized in that
The raw material includes: that 35 parts of modified pitch, 18 parts of butadiene-styrene rubber, vinyl pyrrolidone-vinyl acetate are total by weight 18 parts of aggressiveness, 6 parts of polyethylene glycol oxide, 3 parts of polyvinyl alcohol, 12 parts of cellulose acetate, 0.5 part of C_4 hydrocarbon, 6 parts of tackifier, propylene 4 parts of sour methyl esters, 5 parts of softening agent, 5 parts of different tridecyl alcohol phosphate ester and 8 parts of diisooctyl phthalate.
7. a kind of high-polymer strong according to claim 4 intersects film reaction type adhesive waterproof coil, which is characterized in that institute Tackifier are stated, are made of pitch tackifier GXJ- I and terpene resin T-110, GXJ- I and terpene resin T-110 mass ratio are 3: 7。
8. a kind of high-polymer strong according to claim 4 intersects film reaction type adhesive waterproof coil, which is characterized in that
The different tridecyl alcohol phosphate ester, pH value 3.3-4.1, solid content 96.5-99.5%.
9. a kind of high-polymer strong according to claim 4 intersects film reaction type adhesive waterproof coil, which is characterized in that
The C_4 hydrocarbon, mono-olefin content accounting are 2.2-10.6%, and diene content accounting is 6.8-22.9%, methyl tertbutyl Ether content is 1.5-12.4%, and sulfur content is lower than 5ppm.
10. a kind of high-polymer strong according to claim 3 intersects film reaction type adhesive waterproof coil, which is characterized in that The high-polymer strong intersects film reaction type adhesive waterproof coil, and the peel strength between material and coiled material is 3.1N/mm, coiled material with Peel strength between aluminium is 3.7N/mm, and wear-resistant power reaches 10028rad.
CN201810501539.3A 2018-05-23 2018-05-23 A kind of high-polymer strong intersects film reaction type adhesive waterproof coil and preparation method thereof Withdrawn CN110527307A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112708159A (en) * 2020-12-22 2021-04-27 江苏求实塑业有限公司 High-performance stretch-resistant nano modified strong cross membrane and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112708159A (en) * 2020-12-22 2021-04-27 江苏求实塑业有限公司 High-performance stretch-resistant nano modified strong cross membrane and preparation method thereof

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Application publication date: 20191203

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