阅读说明：本技术 一种具有高抗冲击强度性能的pe管的制备方法 (Preparation method of PE pipe with high impact strength performance ) 是由 丁柳朋 于 2020-12-25 设计创作，主要内容包括：本发明公开了一种具有高抗冲击强度性能的PE管的制备方法,包括以下步骤：步骤一,PE基体的制备：将10-20份PE塑料进行融化处理,融化温度为185-195℃,融化10-20min,然后向其中加入5-10份界面改性剂,然后进行搅拌处理,搅拌转速为20-100r/min,搅拌10-20min,然后进行双螺杆挤出,得到PE基体。本发明PE基体采用PE塑料进行融化处理,然后通过界面改性剂进行界面相容处理,界面改性剂采用短切玻璃纤维先对其羟基化处理,然后在稀土液与淀粉液中共混改性,从而改善其亲有机、亲无机性能。(The invention discloses a preparation method of a PE pipe with high impact strength performance, which comprises the following steps: step one, preparing a PE matrix: melting 10-20 parts of PE plastic at the temperature of 185-195 ℃ for 10-20min, adding 5-10 parts of interface modifier, stirring at the rotation speed of 20-100r/min for 10-20min, and extruding by using a double screw to obtain the PE matrix. The PE matrix is subjected to melting treatment by adopting PE plastic, then is subjected to interface compatibility treatment by adopting an interface modifier, and the interface modifier is subjected to hydroxylation treatment by adopting chopped glass fiber, and then is mixed and modified in rare earth liquid and starch liquid, so that the organophilic and inotropic properties of the PE matrix are improved.)

1. A preparation method of a PE pipe with high impact strength performance is characterized by comprising the following steps:

step one, preparing a PE matrix: melting 10-20 parts of PE plastic at the temperature of 185-195 ℃ for 10-20min, adding 5-10 parts of an interface modifier, stirring at the stirring speed of 20-100r/min for 10-20min, and extruding by using a double screw to obtain a PE matrix;

the preparation method of the interface modifier comprises the following steps:

s1: sending the chopped glass fiber into concentrated sulfuric acid for oxidation treatment, then washing with water, and sending into a coupling agent for coupling treatment to obtain hydroxylated chopped glass fiber;

s2: adding starch into 30-50 times volume of deionized water, stirring at 55-65 ℃ and 200-300rpm for 25-35min, adding sodium bicarbonate, heating to 85-95 ℃, and continuing stirring at 500-600rpm for gelatinization for 20-30min to obtain starch solution;

s3: sending lanthanum chloride rare earth into a proton irradiation box for activation irradiation, wherein the irradiation power is 200-300W, the irradiation time is 10-20min, then adding a coupling agent KH560, stirring for 20-30min, and the stirring speed is 150-250r/min to obtain rare earth liquid;

s4: adding the rare earth liquid into the starch liquid in S2, mixing and stirring, adding the hydroxylated chopped glass fiber in S1, adding dibutyltin dilaurate, heating to 124-;

step two, modifying brucite: grinding and refining brucite, then adding the ground brucite into deionized water with the volume 5-10 times of that of the brucite, dispersing for 10-15min at 82-85 ℃ and 1100rpm under 1000-plus-one pressure to obtain suspension, then adding 3-5 parts of methyl methacrylate, continuing to stir for 20-30min, adding a stable coating agent after stirring is finished, continuing to perform ultrasonic dispersion for 10-20min, and obtaining modified brucite with the ultrasonic power of 100-plus-200W;

step three, mixing material treatment: feeding the PE matrix, the modified brucite and the dispersing agent in the step one into a mixer for mixing and stirring, wherein the mixing speed is 100-200r/min, and the mixing time is 20-30min, so as to obtain a mixed material;

step four, extrusion molding treatment: and (3) feeding the mixed material into a double-screw extruder for extrusion, and then feeding the mixed material into a die for hot-pressing and shaping to obtain the PE pipe.

2. The method for preparing PE pipe with high impact strength according to claim 1, wherein the stable coating agent is prepared by: adding sodium silicate into nano calcium carbonate, then adding a coupling agent, then sending into a reaction kettle with the temperature of 130-134 ℃, preserving heat, standing for 40-50min, cooling, filtering, and drying at the temperature of 55-60 ℃ for 15-25min to obtain the stable coating agent.

3. The method for preparing the PE pipe with high impact strength as claimed in claim 2, wherein the mass ratio of the sodium silicate to the nano calcium carbonate to the coupling agent is (5-9): 1-3): 1.

4. The method for preparing the PE pipe with high impact strength performance according to claim 3, wherein the mass ratio of the sodium silicate to the nano calcium carbonate to the coupling agent is 7:2: 1.

5. The method for preparing a PE pipe with high impact strength as claimed in claim 1, wherein the dispersant is prepared by: adding terephthalic acid into an N, N-dimethylformamide solvent, then adding acetic acid to adjust the pH of the solution to 5.5-6.5, then adding a bisphenol A epoxy resin emulsion and a promoter, stirring for 20-30min at the stirring speed of 50-150r/min, and obtaining the dispersing agent after the stirring is finished.

6. The process for preparing PE pipe with high impact strength according to claim 5, wherein the promoter is epichlorohydrin.

7. The method for preparing a PE pipe with high impact strength according to claim 1, wherein the hot press forming is performed at a pressure of 5-10MPa and a temperature of 55-65 ℃, and after the hot press forming is completed, the PE pipe is cooled to room temperature.

8. The method for preparing PE pipe with high impact strength according to claim 7, wherein the pressure for hot press forming is 7.5MPa and the temperature is 60 ℃.

Technical Field

The invention relates to the technical field of metal surface treatment, in particular to a preparation method of a PE pipe with high impact strength performance.

Background

PE is polyethylene plastic, the most basic plastic, plastic bags, preservative films and the like are PE, and HDPE is a nonpolar thermoplastic resin with high crystallinity. The appearance of the original HDPE is milky white, and the micro-thin section is semitransparent to a certain degree. PE has excellent resistance to most domestic and industrial chemicals. The PE pipe includes a medium density polyethylene pipe and a high density polyethylene pipe. The series was classified according to wall thickness as SDR11 and SDR 17.6. The former is suitable for conveying gaseous artificial gas, natural gas and liquefied petroleum gas, and the latter is mainly used for conveying natural gas. Compared with a steel pipe, the construction process is simple, has certain flexibility, and is mainly not used for anticorrosion treatment, so that a large number of working procedures are saved. The disadvantage is that the device is not as good as steel pipe, the safety space of thermal heating is specially paid attention to in construction, and the device can not be exposed in the sun in the air and is sensitive to chemical substances, thus preventing the sewage pipeline from being leaked to cause damage.

In order to change the impact strength of the existing PE pipe, a large amount of impact resistant agent is added into the PE pipe material, and the impact resistant agent has poor compatibility with raw materials in the PE pipe material, so that the impact strength performance of the product is influenced.

Therefore, the invention provides a preparation method of the PE pipe with the impact strength performance.

Disclosure of Invention

The present invention is directed to a method for preparing a PE pipe having high impact strength properties to solve the problems set forth in the background art.

In order to achieve the purpose, the invention provides the following technical scheme:

the invention provides a preparation method of a PE pipe with impact strength performance, which comprises the following steps:

step one, preparing a PE matrix: melting 10-20 parts of PE plastic at the temperature of 185-195 ℃ for 10-20min, adding 5-10 parts of an interface modifier, stirring at the stirring speed of 20-100r/min for 10-20min, and extruding by using a double screw to obtain a PE matrix;

the preparation method of the interface modifier comprises the following steps:

s1: sending the chopped glass fiber into concentrated sulfuric acid for oxidation treatment, then washing with water, and sending into a coupling agent for coupling treatment to obtain hydroxylated chopped glass fiber;

s2: adding starch into 30-50 times volume of deionized water, stirring at 55-65 ℃ and 200-300rpm for 25-35min, adding sodium bicarbonate, heating to 85-95 ℃, and continuing stirring at 500-600rpm for gelatinization for 20-30min to obtain starch solution;

s3: sending lanthanum chloride rare earth into a proton irradiation box for activation irradiation, wherein the irradiation power is 200-300W, the irradiation time is 10-20min, then adding a coupling agent KH560, stirring for 20-30min, and the stirring speed is 150-250r/min to obtain rare earth liquid;

s4: adding the rare earth liquid into the starch liquid in S2, mixing and stirring, adding the hydroxylated chopped glass fiber in S1, adding dibutyltin dilaurate, heating to 124-;

step two, modifying brucite: grinding and refining brucite, then adding the ground brucite into deionized water with the volume 5-10 times of that of the brucite, dispersing for 10-15min at 82-85 ℃ and 1100rpm under 1000-plus-one pressure to obtain suspension, then adding 3-5 parts of methyl methacrylate, continuing to stir for 20-30min, adding a stable coating agent after stirring is finished, continuing to perform ultrasonic dispersion for 10-20min, and obtaining modified brucite with the ultrasonic power of 100-plus-200W;

step three, mixing material treatment: feeding the PE matrix, the modified brucite and the dispersing agent in the step one into a mixer for mixing and stirring, wherein the mixing speed is 100-200r/min, and the mixing time is 20-30min, so as to obtain a mixed material;

step four, extrusion molding treatment: and (3) feeding the mixed material into a double-screw extruder for extrusion, and then feeding the mixed material into a die for hot-pressing and shaping to obtain the PE pipe.

Preferably, the preparation method of the stable coating agent comprises the following steps: adding sodium silicate into nano calcium carbonate, then adding a coupling agent, then sending into a reaction kettle with the temperature of 130-134 ℃, preserving heat, standing for 40-50min, cooling, filtering, and drying at the temperature of 55-60 ℃ for 15-25min to obtain the stable coating agent.

Preferably, the mass ratio of the sodium silicate to the nano calcium carbonate to the coupling agent is (5-9): 1-3): 1.

Preferably, the mass ratio of the sodium silicate to the nano calcium carbonate to the coupling agent is 7:2: 1.

Preferably, the preparation method of the dispersant is as follows: adding terephthalic acid into an N, N-dimethylformamide solvent, then adding acetic acid to adjust the pH of the solution to 5.5-6.5, then adding a bisphenol A epoxy resin emulsion and a promoter, stirring for 20-30min at the stirring speed of 50-150r/min, and obtaining the dispersing agent after the stirring is finished.

Preferably, the accelerant is epichlorohydrin.

Preferably, the hot-press shaping is carried out by adopting the pressure of 5-10MPa and the temperature of 55-65 ℃, and after shaping, the product is cooled to room temperature.

Preferably, the pressure of the hot-press shaping is 7.5MPa, and the temperature is 60 ℃.

Compared with the prior art, the invention has the following beneficial effects:

the PE matrix is subjected to melting treatment by adopting PE plastic, then interface compatibility treatment is carried out by adopting an interface modifier, the interface modifier is subjected to hydroxylation treatment by adopting chopped glass fibers, and then the hydroxylated glass fibers are mixed and modified in rare earth liquid and starch liquid, so that the organophilic and inotropic properties of the modified PE matrix are improved, the addition of the starch liquid can play an auxiliary role, the contact effect of the chopped fibers and the rare earth liquid can be improved, the viscosity of the solution can be improved by the starch liquid, the bonding strength between the solution and the starch liquid is improved, the wetting effect of the rare earth liquid on the chopped fibers is improved, the chopped glass fibers are distributed in the PE matrix in a fiber shape after being treated, the strength property of the product can be obviously improved, and the interface compatibility of the product is improved;

the modified brucite can be uniformly dispersed in a matrix by grinding and refining, so that the strength performance of the product is further improved, meanwhile, the modified brucite is coated by the synergistic combination of sodium silicate, nano calcium carbonate and a coupling agent in a stable coating agent, so that the stability of the brucite in the matrix is improved, the nano calcium carbonate can play a role in enhancing the dispersibility of the brucite in a synergistic manner, and the coupling agent enhances the organophilic property of the brucite;

the dispersing agent is prepared from terephthalic acid, N-dimethylformamide solvent, bisphenol A epoxy resin emulsion and other raw materials, and can enhance the blending contact effect between PE plastic and modified brucite, because the bisphenol A epoxy resin emulsion can play an intermediate connection effect, the modified brucite is further connected with a matrix, and meanwhile, the terephthalic acid, N-dimethylformamide solvent further moistens the raw materials of the product, so that the mutual matching reaction between the raw materials of the product is facilitated, the integral forming effect of the product is better, the agglomeration force of the product is stronger, and the impact strength can be obviously improved.

Detailed Description

The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, 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.

Example 1:

the preparation method of the PE pipe with high impact strength performance of this embodiment includes the following steps:

step one, preparing a PE matrix: melting 10 parts of PE plastic at 185 ℃ for 10min, adding 5 parts of interface modifier, stirring at 20r/min for 10min, and extruding by using a double screw to obtain a PE matrix;

the preparation method of the interface modifier comprises the following steps:

s1: sending the chopped glass fiber into concentrated sulfuric acid for oxidation treatment, then washing with water, and sending into a coupling agent for coupling treatment to obtain hydroxylated chopped glass fiber;

s2: adding starch into 30 times of deionized water, stirring at 55 deg.C and 200rpm for 25min, adding sodium bicarbonate, heating to 85 deg.C, stirring at 500rpm, and gelatinizing for 20min to obtain starch solution;

s3: feeding lanthanum chloride rare earth into a proton irradiation box for activation irradiation, wherein the irradiation power is 200W, the irradiation time is 10min, then adding a coupling agent KH560, stirring for 20min, and stirring at the rotation speed of 150r/min to obtain rare earth liquid;

s4: adding the rare earth liquid into the starch liquid in S2, mixing and stirring, adding the hydroxylated chopped glass fiber in S1, adding dibutyltin dilaurate, heating to 124 ℃, stirring at a high speed for 2 hours, naturally cooling to room temperature, washing with water, and drying to obtain an interface modifier;

step two, modifying brucite: grinding and refining brucite, then adding the ground brucite into deionized water with the volume 5 times that of the brucite, dispersing for 10min at 82 ℃ and 1000rpm to obtain a suspension, then adding 3 parts of methyl methacrylate, continuing to stir for 20min, adding a stable coating agent after stirring is finished, continuing to perform ultrasonic dispersion for 10min, wherein the ultrasonic power is 100W, and obtaining modified brucite;

step three, mixing material treatment: feeding the PE matrix, the modified brucite and the dispersing agent in the step one into a mixer for mixing and stirring, wherein the mixing speed is 100r/min, and the mixing time is 20min, so as to obtain a mixed material;

step four, extrusion molding treatment: and (3) feeding the mixed material into a double-screw extruder for extrusion, and then feeding the mixed material into a die for hot-pressing and shaping to obtain the PE pipe.

The preparation method of the stable coating agent of the embodiment comprises the following steps: adding sodium silicate into nano calcium carbonate, then adding a coupling agent, then sending into a reaction kettle at 130 ℃, preserving heat, standing for 40min, cooling, filtering, and drying at 55 ℃ for 15min to obtain the stable coating agent.

The mass ratio of the sodium silicate, the nano calcium carbonate and the coupling agent in the embodiment is 5:1: 1.

The preparation method of the dispersant of the embodiment comprises the following steps: adding terephthalic acid into an N, N-dimethylformamide solvent, adding acetic acid to adjust the pH of the solution to 5.5, then adding a bisphenol A epoxy resin emulsion and a promoter, stirring for 20min at the stirring speed of 50r/min, and obtaining the dispersing agent after the stirring is finished.

The accelerator in this example was epichlorohydrin.

The hot press forming of this embodiment is performed by using a pressure of 5MPa and a temperature of 55 ℃, and after the forming is completed, the molded product is cooled to room temperature.

Example 2:

the preparation method of the PE pipe with high impact strength performance of this embodiment includes the following steps:

step one, preparing a PE matrix: melting 20 parts of PE plastic at the temperature of 195 ℃ for 20min, adding 10 parts of interface modifier, stirring at the rotation speed of 100r/min for 20min, and extruding by using a double screw to obtain a PE matrix;

the preparation method of the interface modifier comprises the following steps:

s1: sending the chopped glass fiber into concentrated sulfuric acid for oxidation treatment, then washing with water, and sending into a coupling agent for coupling treatment to obtain hydroxylated chopped glass fiber;

s2: adding starch into deionized water 50 times of the volume of the starch, stirring at 65 ℃ and 300rpm for 35min, then adding sodium bicarbonate, heating to 95 ℃, and continuing stirring at 600rpm for gelatinization for 30min to obtain a starch solution;

s3: sending lanthanum chloride rare earth into a proton irradiation box for activation irradiation, wherein the irradiation power is 300W, the irradiation time is 20min, then adding a coupling agent KH560, stirring for 30min, and the stirring rotating speed is 250r/min to obtain rare earth liquid;

s4: adding the rare earth liquid into the starch liquid in S2, mixing and stirring, adding the hydroxylated chopped glass fiber in S1, adding dibutyltin dilaurate, heating to 130 ℃, stirring at a high speed for 2 hours, naturally cooling to room temperature, washing with water, and drying to obtain an interface modifier;

step two, modifying brucite: grinding and refining brucite, then adding the ground brucite into deionized water with the volume being 10 times that of the brucite, dispersing for 15min at 85 ℃ and 1100rpm to obtain a suspension, then adding 5 parts of methyl methacrylate, continuing to stir for 30min, adding a stable coating agent after stirring is finished, continuing to perform ultrasonic dispersion for 20min, wherein the ultrasonic power is 200W, and obtaining modified brucite;

step three, mixing material treatment: feeding the PE matrix, the modified brucite and the dispersing agent in the step one into a mixer for mixing and stirring, wherein the mixing speed is 200r/min, and the mixing time is 30min, so as to obtain a mixed material;

step four, extrusion molding treatment: and (3) feeding the mixed material into a double-screw extruder for extrusion, and then feeding the mixed material into a die for hot-pressing and shaping to obtain the PE pipe.

The preparation method of the stable coating agent of the embodiment comprises the following steps: adding sodium silicate into nano calcium carbonate, then adding a coupling agent, then sending into a reaction kettle at 134 ℃, preserving heat, standing for 50min, cooling, filtering, and drying at 60 ℃ for 25min to obtain the stable coating agent.

The mass ratio of the sodium silicate, the nano calcium carbonate and the coupling agent in the embodiment is 9:3: 1.

The preparation method of the dispersant of the embodiment comprises the following steps: adding terephthalic acid into an N, N-dimethylformamide solvent, adding acetic acid to adjust the pH of the solution to 6.5, then adding a bisphenol A epoxy resin emulsion and a promoter, stirring for 30min at the stirring speed of 150r/min, and obtaining the dispersing agent after the stirring is finished.

The accelerator in this example was epichlorohydrin.

The hot press forming of this example was carried out under a pressure of 10MPa and at a temperature of 65 ℃, and after the forming was completed, the steel sheet was cooled to room temperature.

Example 3:

the preparation method of the PE pipe with high impact strength performance of this embodiment includes the following steps:

step one, preparing a PE matrix: melting 15 parts of PE plastic at 190 ℃ for 15min, adding 5-10 parts of an interface modifier, stirring at a stirring speed of 60r/min for 15min, and performing double-screw extrusion to obtain a PE matrix;

the preparation method of the interface modifier comprises the following steps:

s1: sending the chopped glass fiber into concentrated sulfuric acid for oxidation treatment, then washing with water, and sending into a coupling agent for coupling treatment to obtain hydroxylated chopped glass fiber;

s2: adding starch into deionized water 40 times of the volume of the starch, stirring at 60 ℃ and 250rpm for 30min, then adding sodium bicarbonate, heating to 90 ℃, and continuing stirring at 550rpm for gelatinization for 25min to obtain a starch solution;

s3: feeding lanthanum chloride rare earth into a proton irradiation box for activation irradiation, wherein the irradiation power is 250W, the irradiation time is 15min, then adding a coupling agent KH560, stirring for 25min, and stirring at the rotation speed of 200r/min to obtain rare earth liquid;

s4: adding the rare earth liquid into the starch liquid in S2, mixing and stirring, adding the hydroxylated chopped glass fiber in S1, adding dibutyltin dilaurate, heating to 126 ℃, stirring at a high speed for 2 hours, naturally cooling to room temperature, washing with water, and drying to obtain an interface modifier;

step two, modifying brucite: grinding and refining the brucite, adding the ground brucite into deionized water with the volume 5-10 times of that of the brucite, dispersing for 12.5min at 83.5 ℃ and 1100rpm under 1000-;

step three, mixing material treatment: feeding the PE matrix, the modified brucite and the dispersing agent in the step one into a mixer for mixing and stirring, wherein the mixing speed is 150r/min, and the mixing time is 25min, so as to obtain a mixed material;

step four, extrusion molding treatment: and (3) feeding the mixed material into a double-screw extruder for extrusion, and then feeding the mixed material into a die for hot-pressing and shaping to obtain the PE pipe.

The preparation method of the stable coating agent of the embodiment comprises the following steps: adding sodium silicate into nano calcium carbonate, then adding a coupling agent, then sending into a reaction kettle at 132 ℃, preserving heat, standing for 45min, cooling, filtering, and drying at 57.5 ℃ for 20min to obtain the stable coating agent.

The mass ratio of the sodium silicate, the nano calcium carbonate and the coupling agent in the embodiment is 7:2: 1.

The preparation method of the dispersant of the embodiment comprises the following steps: adding terephthalic acid into an N, N-dimethylformamide solvent, adding acetic acid to adjust the pH of the solution to 6.0, then adding a bisphenol A epoxy resin emulsion and a promoter, stirring for 25min at the stirring speed of 75r/min, and obtaining the dispersing agent after the stirring is finished.

The accelerator in this example was epichlorohydrin.

The hot press forming of this embodiment is performed by using a pressure of 7.5MPa and a temperature of 60 ℃, and after the forming is completed, the product is cooled to room temperature.

Comparative example 1:

the materials and preparation process were substantially the same as those of example 3, except that no dispersant was added.

Comparative example 2:

a PE pipe on the market is used.

And (4) adopting a universal material testing machine to carry out product impact resistance test and testing impact strength.

Group of	Impact strength (MPa)
		Example 1	61
Example 2	63
		Example 3	68
Comparative example 1	52
		Comparative example 2	37

Examples 1-3 and comparative examples 1-2 show that the impact strength of the PE pipe of the present invention is higher than 61MPa, which is significantly improved compared to the products on the market.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.