阅读说明：本技术 一种自粘防水卷材及其制备方法 (Self-adhesive waterproof coiled material and preparation method thereof ) 是由 梁子双 梁本树 陆子明 于 2021-07-12 设计创作，主要内容包括：本发明公开了一种自粘防水卷材及其制备方法,属于建筑防水材料技术领域,解决现有防水卷材耐老化性能不好的技术问题。该自粘防水卷材包括如下重量份原料：基质沥青55-65份、丁腈橡胶粉17-23份、填料10-15份、石蜡4-6份、防老剂2-5份,本发明还公开了自粘防水卷材的制备方法,先将基质沥青和丁腈橡胶密炼制成胶料,再将石蜡、填料和防老剂加入石脑油混合制成复合助剂,之后将胶料和复合助剂高速剪切,最后倒入模具成型、辊压、冷却、收卷制成自粘防水卷材；制备的防老剂的分子上含有9个亚氨基,具有良好的防老化性能,并与石蜡混合加入胶料中,石蜡携带部分防老剂在表面形成蜡膜,具有优异的防老化性能。(The invention discloses a self-adhesive waterproof coiled material and a preparation method thereof, belongs to the technical field of building waterproof materials, and solves the technical problem that the existing waterproof coiled material is poor in aging resistance. The self-adhesive waterproof roll comprises the following raw materials in parts by weight: 55-65 parts of matrix asphalt, 17-23 parts of nitrile rubber powder, 10-15 parts of filler, 4-6 parts of paraffin and 2-5 parts of anti-aging agent, and the invention also discloses a preparation method of the self-adhesive waterproof coiled material, wherein the matrix asphalt and the nitrile rubber are banburied to prepare a sizing material, then the paraffin, the filler and the anti-aging agent are added into naphtha to be mixed to prepare a composite auxiliary agent, then the sizing material and the composite auxiliary agent are sheared at high speed, and finally the mixture is poured into a mould to be molded, rolled, cooled and rolled to prepare the self-adhesive waterproof coiled material; the prepared anti-aging agent contains 9 imino groups on molecules, has good anti-aging performance, is mixed with paraffin and added into rubber, and the paraffin carries part of the anti-aging agent to form a wax film on the surface, so that the anti-aging agent has excellent anti-aging performance.)

1. The self-adhesive waterproof roll is characterized by comprising the following raw materials in parts by weight: 55-65 parts of matrix asphalt, 17-23 parts of nitrile rubber powder, 10-15 parts of filler, 4-6 parts of paraffin and 2-5 parts of anti-aging agent;

the anti-aging agent is prepared by the following steps:

step A1: adding p-phenylenediamine and aniline into a reaction kettle, removing air in the reaction kettle, filling boron trichloride until the pressure is 1.5-1.9MPa, heating to 320-;

step A2: adding melamine and dimethyl sulfoxide into a reaction kettle, stirring and dissolving, adding epoxy chloropropane into the reaction kettle, heating to 48-55 ℃ under the protection of dry nitrogen, stirring and reacting for 7-9h, then heating to 120-180 ℃, stirring and reacting for 1-1.5h, separating by using deionized water, taking an organic layer, and removing water by using calcium oxide to obtain an intermediate 2;

step A3: and adding the intermediate 1, the intermediate 2 and tetrahydrofuran into a reaction kettle, controlling the temperature to be 50-65 ℃, stirring for reacting for 18-24h, and carrying out rotary evaporation under reduced pressure to remove the tetrahydrofuran to obtain the anti-aging agent.

2. The self-adhesive waterproof roll according to claim 1, wherein in the step A1, the molar ratio of the phenylenediamine to the aniline is 1:1.

3. The self-adhesive waterproof roll according to claim 1, wherein in the step A2, the molar ratio of the melamine to the epichlorohydrin is 1: 1.05-1.1.

4. The self-adhesive waterproof roll according to claim 1, wherein in the step A3, the dosage ratio of the intermediate 1 to the intermediate 2 is 17.5 mL: 9.1-10.3 mL.

5. The self-adhesive waterproof roll according to claim 1, wherein the filler is one or more of lime powder, coal ash powder and talcum powder which are mixed in any proportion.

6. A preparation method of a self-adhesive waterproof roll is characterized by comprising the following steps:

step S1: adding the matrix asphalt into an internal mixer, controlling the temperature to be 220-180 ℃, heating the matrix asphalt to be molten, adding the nitrile-butadiene rubber powder into the internal mixer, stirring and blending for 30-50min, and then adding the asphalt oil into the internal mixer to adjust the penetration degree of the mixture to be 170-180 to prepare a rubber material;

step S2: adding paraffin, filler, anti-aging agent and naphtha into a stirrer, heating to 65-70 ℃, and stirring for 1-2 hours to obtain a composite auxiliary agent;

step S3: mixing the composite auxiliary agent and the sizing material, adding the mixture into a high-shear emulsifying machine, controlling the temperature to be 180 ℃ and 200 ℃, and performing high-speed shearing for 30-40min to obtain a waterproof base material;

step S4: spreading glass cloth at the bottom of the forming mold, pouring the waterproof base material into the mold, rolling, cooling, laminating and rolling to obtain the self-adhesive waterproof roll.

Technical Field

The invention belongs to the technical field of building waterproof materials, and particularly relates to a self-adhesive waterproof roll and a preparation method thereof.

Background

The waterproof coiled material is mainly used for building walls, roofs, tunnels, highways, refuse landfills and the like, can be curled into a roll-shaped flexible building material product for resisting external rainwater and underground water leakage, is used as a leakage-free connection between an engineering foundation and a building, is a waterproof first barrier of the whole engineering, and plays a vital role in the whole engineering.

Asphalt belongs to a hydrophobic material, is impermeable and almost insoluble in water, is widely applied to waterproof materials, but is easy to flow at high temperature, and is easy to age and crack on the surface when being exposed to outdoor sunlight for a long time, so that the waterproof performance is seriously influenced.

Disclosure of Invention

The invention aims to provide a self-adhesive waterproof roll and a preparation method thereof.

The technical problems to be solved by the invention are as follows: the prior waterproof coiled material has the technical problem of poor aging resistance.

The purpose of the invention can be realized by the following technical scheme:

a self-adhesive waterproof coiled material comprises 55-65 parts of matrix asphalt, 17-23 parts of nitrile rubber powder, 10-15 parts of filler, 4-6 parts of paraffin and 2-5 parts of anti-aging agent;

an antioxidant prepared by the following steps:

step A1: adding p-phenylenediamine and aniline into a reaction kettle, vacuumizing the reaction kettle to 300-1.9 Pa, filling boron trichloride into the reaction kettle until the pressure is 1.5-1.9MPa, heating the reaction system to 320-360 ℃, controlling the stirring speed to 800-1000r/min, and stirring for 15-20h to obtain an intermediate 1;

the specific reaction is as follows:

step A2: adding melamine and dimethyl sulfoxide into a reaction kettle, stirring until the melamine is dissolved, adding epoxy chloropropane into the reaction kettle, heating to 48-55 ℃ under the protection of dry nitrogen, setting the stirring speed to be 200-fold organic silicon at 300r/min, reacting for 7-9h, then heating to 120-fold organic silicon at 180 ℃, increasing the rotation speed to be 700-fold organic silicon at 800r/min, reacting for 1-1.5h, washing the reaction liquid with deionized water for 2-3 times, and then using calcium oxide to remove water to prepare an intermediate 2;

the specific reaction is as follows:

step A3: and adding the intermediate 1, the intermediate 2 and tetrahydrofuran into a reaction kettle, controlling the temperature to be 50-65 ℃, stirring at the speed of 200-250r/min, stirring for reacting for 18-24h, and carrying out reduced pressure rotary evaporation to remove the tetrahydrofuran to obtain the anti-aging agent.

The specific reaction is as follows:

in step A1, phenylenediamine and aniline are used in a molar ratio of 1:1.

Further, in the step A2, before the dimethyl sulfoxide is used, water is removed through vacuum distillation, and the molar ratio of the melamine to the epichlorohydrin is 1: 1.05-1.1.

Further, in step a3, the ratio of the amounts of intermediate 1 and intermediate 2 was 17.5 mL: 9.1-10.3 mL.

Furthermore, the filler is one or a mixture of more of lime powder, coal ash powder and talcum powder in any proportion.

A preparation method of a self-adhesive waterproof roll comprises the following steps:

step S1: adding the matrix asphalt into an internal mixer, controlling the temperature to be 220-180 ℃, heating the matrix asphalt to be molten, adding the nitrile-butadiene rubber powder into the internal mixer, keeping the temperature unchanged, controlling the stirring speed to be 180-240r/min, blending for 30-50min, and then adding the asphalt oil into the internal mixer to adjust the penetration degree of the mixture to be 170-180 to prepare a rubber material;

step S2: adding paraffin, filler, anti-aging agent and naphtha into a stirrer, heating to 65-70 ℃, controlling the stirring speed to be 300-400r/min, and stirring for 1-2h to obtain a composite auxiliary agent, wherein the dosage of the naphtha is 30% of the total mass of the paraffin, the filler and the anti-aging agent;

step S3: mixing the composite auxiliary agent and the sizing material, adding the mixture into a high-shear emulsifying machine, controlling the temperature to be 180-;

step S4: spreading glass cloth at the bottom of the forming mold, pouring the waterproof base material into the mold, rolling, cooling, laminating and rolling to obtain the self-adhesive waterproof roll.

The invention has the beneficial effects that:

1. the invention provides a self-adhesive waterproof coiled material and a preparation method thereof, the waterproof coiled material takes matrix asphalt and nitrile rubber as main raw materials to be blended, and the powdered rubber is filled in the asphalt to increase the strength of the asphalt under the high-temperature working condition; this waterproofing membrane one side adopts glass cloth as base cloth, and another side tectorial membrane is handled, tears the tectorial membrane during the use and compacts on the working face, pitch and working face direct contact, and butadiene acrylonitrile rubber and pitch have good adhesion properties for waterproofing membrane has the self-adhesion characteristic, need not to use the adhesive.

2. The invention has prepared an anti-aging agent in the course of preparing the self-adhered waterproofing membrane, this anti-aging agent takes phenylenediamine and aniline as raw materials, boron trichloride is the catalyst, and pack to react under the high-pressure condition with boron trichloride and make midbody 1, react with epoxy chloropropane with melamine, connect epoxy group on melamine, make midbody 2, take the ring opening reaction with midbody 2 epoxy group on amino on midbody 1, make anti-aging agent, this anti-aging agent contains 9 imino on every molecule, have good anti-aging performance, in addition, in the course of preparing, mix anti-aging agent and paraffin and add into sizing material, the paraffin carries some anti-aging agent to move to the surface layer of the sizing material through the way of molecular motion, form a layer of wax film with high anti-aging agent content on the surface, separate the internal material from outside on the one hand, hinder the coiled material from being corroded, on the other hand, the wax film with high anti-aging agent content is aged first, so that the aging resistance of the coiled material is improved.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In the examples:

the filler comprises lime powder, coal ash powder and talcum powder, the materials are finely ground and sieved by a 300-mesh screen, and the materials are mixed according to the mass ratio of 1:1.15: 0.9.

The matrix asphalt is 70# road asphalt.

Example 1

The embodiment of the preparation of the anti-aging agent specifically comprises the following steps:

step A1: adding p-phenylenediamine and aniline into a reaction kettle according to the molar ratio of 1:1, vacuumizing the reaction kettle to 500Pa, filling boron trichloride into the reaction kettle until the pressure is 1.5MPa, heating the reaction system to 320 ℃, controlling the stirring speed to be 800r/min, and stirring for 15 hours to obtain an intermediate 1;

step A2: taking dimethyl sulfoxide, distilling under reduced pressure to remove water, taking melamine and dimethyl sulfoxide according to the dosage ratio of 5.5 g: adding 20mL of the mixture into a reaction kettle, stirring until melamine is dissolved, adding epoxy chloropropane into the reaction kettle according to the molar ratio of the melamine to the epoxy chloropropane of 1:1.05, heating to 48 ℃ under the protection of dry nitrogen, setting the stirring speed to be 200r/min, reacting for 7 hours, heating to 120 ℃, increasing the rotating speed to be 700r/min, reacting for 1 hour, washing the reaction solution for 2 times by using deionized water, and removing water by using calcium oxide to obtain an intermediate 2;

step A3: taking the intermediate 1, the intermediate 2 and tetrahydrofuran according to the dosage ratio of 17.5 mL: 9.1 mL: adding 30mL of the mixture into a reaction kettle, controlling the temperature to be 50 ℃, stirring at the speed of 200r/min, stirring for reacting for 18 hours, and carrying out reduced pressure rotary evaporation to remove tetrahydrofuran to obtain the anti-aging agent.

Example 2

The embodiment of the preparation of the anti-aging agent specifically comprises the following steps:

step A1: adding p-phenylenediamine and aniline into a reaction kettle according to the dosage molar ratio of 1:1, vacuumizing the reaction kettle to 400Pa, filling boron trichloride into the reaction kettle until the pressure is 1.7MPa, heating the reaction system to 350 ℃, controlling the stirring speed to be 900r/min, and stirring for 17 hours to obtain an intermediate 1;

step A2: taking dimethyl sulfoxide, distilling under reduced pressure to remove water, taking melamine and dimethyl sulfoxide according to the dosage ratio of 5.5 g: adding 20mL of the mixture into a reaction kettle, stirring until melamine is dissolved, adding epoxy chloropropane into the reaction kettle according to the molar ratio of the melamine to the epoxy chloropropane of 1:1.1, heating to 50 ℃ under the protection of dry nitrogen, setting the stirring speed to be 300r/min, reacting for 9 hours, heating to 150 ℃, increasing the rotating speed to be 800r/min, reacting for 1.5 hours, washing the reaction solution for 2 times by using deionized water, and removing water by using calcium oxide to obtain an intermediate 2;

step A3: taking the intermediate 1, the intermediate 2 and tetrahydrofuran according to the dosage ratio of 17.5 mL: 10mL of: adding 30mL of the antioxidant into a reaction kettle, controlling the temperature to be 55 ℃, stirring at the speed of 200r/min, stirring for reacting for 20 hours, and carrying out reduced pressure rotary evaporation to remove tetrahydrofuran to obtain the antioxidant.

Example 3

The embodiment of the preparation of the anti-aging agent specifically comprises the following steps:

step A1: adding p-phenylenediamine and aniline into a reaction kettle according to the molar ratio of 1:1, vacuumizing the reaction kettle to 300Pa, filling boron trichloride into the reaction kettle until the pressure is 1.9MPa, heating the reaction system to 360 ℃, controlling the stirring speed to be 1000r/min, and stirring for 20 hours to obtain an intermediate 1;

step A2: taking dimethyl sulfoxide, distilling under reduced pressure to remove water, taking melamine and dimethyl sulfoxide according to the dosage ratio of 5.5 g: adding 20mL of the mixture into a reaction kettle, stirring until melamine is dissolved, adding epoxy chloropropane into the reaction kettle according to the molar ratio of the melamine to the epoxy chloropropane of 1:1.1, heating to 55 ℃ under the protection of dry nitrogen, setting the stirring speed to be 300r/min, reacting for 9 hours, heating to 180 ℃, increasing the rotating speed to be 800r/min, reacting for 1.5 hours, washing the reaction solution for 3 times by using deionized water, and removing water by using calcium oxide to obtain an intermediate 2;

step A3: taking the intermediate 1, the intermediate 2 and tetrahydrofuran according to the dosage ratio of 17.5 mL: 10.3 mL: adding 30mL of the antioxidant into a reaction kettle, controlling the temperature to be 65 ℃ and the stirring speed to be 250r/min, stirring for reacting for 24 hours, and carrying out reduced pressure rotary evaporation to remove tetrahydrofuran to obtain the antioxidant.

Example 4

This embodiment prepares a self-adhesion waterproofing membrane, specifically as follows:

a self-adhesive waterproof coiled material comprises 55 parts by weight of matrix asphalt, 17 parts by weight of nitrile rubber powder, 10 parts by weight of filler, 4 parts by weight of paraffin and 2 parts by weight of anti-aging agent;

the preparation process comprises the following steps:

step S1: adding matrix asphalt into an internal mixer, controlling the temperature to be 220 ℃, heating the matrix asphalt to be molten, adding nitrile rubber powder into the internal mixer, keeping the temperature unchanged, controlling the stirring speed to be 180r/min, blending for 30min, then adding asphalt oil into the internal mixer to adjust the needle penetration of the mixture to be 170, and preparing a rubber material;

step S2: adding paraffin, a filler, an anti-aging agent and naphtha into a stirrer, heating to 65 ℃, controlling the stirring speed to be 300r/min, and stirring for 1h to obtain a composite auxiliary agent, wherein the dosage of the naphtha is 30% of the total mass of the paraffin, the filler and the anti-aging agent;

step S3: mixing the composite auxiliary agent and the sizing material, adding the mixture into a high-shear emulsifying machine, controlling the temperature to be 180 ℃, controlling the stirring speed to be 3000r/min, and shearing the mixture for 30min to obtain a waterproof base material;

step S4: spreading glass cloth at the bottom of the forming mold, pouring the waterproof base material into the mold, rolling, cooling, laminating and rolling to obtain the self-adhesive waterproof roll.

Example 5

This embodiment prepares a self-adhesion waterproofing membrane, specifically as follows:

a self-adhesive waterproof coiled material comprises, by weight, 60 parts of matrix asphalt, 20 parts of nitrile rubber powder, 12 parts of filler, 5 parts of paraffin and 4 parts of anti-aging agent;

the preparation process comprises the following steps:

step S1: adding matrix asphalt into an internal mixer, controlling the temperature to be 230 ℃, heating the matrix asphalt to be molten, adding nitrile rubber powder into the internal mixer, keeping the temperature unchanged, controlling the stirring speed to be 200r/min, blending for 40min, then adding asphalt oil into the internal mixer to adjust the needle penetration of the mixture to be 170, and preparing a rubber material;

step S2: adding paraffin, a filler, an anti-aging agent and naphtha into a stirrer, heating to 68 ℃, controlling the stirring speed to be 400r/min, and stirring for 2h to obtain a composite auxiliary agent, wherein the dosage of the naphtha is 30% of the total mass of the paraffin, the filler and the anti-aging agent;

step S3: mixing the composite auxiliary agent and the rubber material, adding the mixture into a high-shear emulsifying machine, controlling the temperature to be 190 ℃, controlling the stirring speed to be 3500r/min, and shearing the mixture for 40min to prepare a waterproof base material;

step S4: spreading glass cloth at the bottom of the forming mold, pouring the waterproof base material into the mold, rolling, cooling, laminating and rolling to obtain the self-adhesive waterproof roll.

Example 6

This embodiment prepares a self-adhesion waterproofing membrane, specifically as follows:

a self-adhesive waterproof coiled material comprises 65 parts by weight of matrix asphalt, 23 parts by weight of nitrile rubber powder, 15 parts by weight of filler, 6 parts by weight of paraffin and 5 parts by weight of anti-aging agent;

the preparation process comprises the following steps:

step S1: adding matrix asphalt into an internal mixer, controlling the temperature to be 250 ℃, heating the matrix asphalt to be molten, adding nitrile rubber powder into the internal mixer, keeping the temperature unchanged, controlling the stirring speed to be 240r/min, blending for 50min, then adding asphalt oil into the internal mixer to adjust the needle penetration of the mixture to be 180, and preparing a rubber material;

step S2: adding paraffin, a filler, an anti-aging agent and naphtha into a stirrer, heating to 70 ℃, controlling the stirring speed to be 400r/min, and stirring for 2h to obtain a composite auxiliary agent, wherein the dosage of the naphtha is 30% of the total mass of the paraffin, the filler and the anti-aging agent;

step S3: mixing the composite auxiliary agent and the rubber material, adding the mixture into a high-shear emulsifying machine, controlling the temperature to be 200 ℃, controlling the stirring speed to be 3500r/min, and shearing the mixture for 40min to prepare a waterproof base material;

step S4: spreading glass cloth at the bottom of the forming mold, pouring the waterproof base material into the mold, rolling, cooling, laminating and rolling to obtain the self-adhesive waterproof roll.

Comparative example 1

The comparative example is the same as the preparation process of example 5, and the antioxidant is replaced by the antioxidant BBPD in the same mass part.

Comparative example 2

The comparative example is the same as the preparation process of example 5, and the anti-aging agent is replaced by the same mass part of paraffin.

Comparative example 3

The comparative example is the same as the example 5, and no antioxidant and no paraffin were added.

The examples 4 to 6 and comparative examples 1 to 3 were subjected to performance tests:

preparing a sample: examples 4-6 and comparative examples 1-3 were made into 200mm by 10mm test specimens;

and (3) aging test: placing the sample in a thermal aging test box, setting the temperature to be 65 ℃, and thermally aging for 1 week;

the test and appearance evaluation of the sample after the heat aging treatment are carried out according to GB/T328.8-2007, and the specific data are shown in the table 1:

TABLE 1

As shown in Table 1, after the aging test, the waterproof roll materials prepared in examples 4-6 have smooth and crack-free surfaces, tensile strength of 17.4-19.7MPa and elongation at break of 654-, a layer of wax film with high anti-aging agent content is formed on the surface, on one hand, the inner material is separated from the outside, and the corrosion of the coiled material is prevented, and on the other hand, the wax film with high anti-aging agent content is firstly aged, so that the aging resistance of the coiled material is improved.

The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.