阅读说明：本技术 一种空气滤材用可复合型热熔胶及其制备方法 (Composite hot melt adhesive for air filter material and preparation method thereof ) 是由 刘济君 于 2021-08-04 设计创作，主要内容包括：本发明提供一种开放时间较长的一种空气滤材用可复合型热熔胶及其制备方法。本发明提供的空气滤材用可复合型热熔胶,按重量份计,由如下成分组成：聚异丁烯5-15份、茂金属催化聚丙烯10-30份、无规聚烯烃20-70份、石油树脂10-45份和抗氧剂0.1-1份；所述聚异丁烯和所述无规聚烯烃的用量比为：1：(4-7),所述聚异丁烯的用量为原料总用量的6％-15％。本发明提供的空气滤材用可复合型热熔胶能够延长产品的开放时间,使热熔胶能够较好的复合其他产品使用。(The invention provides a composite hot melt adhesive for an air filter material with longer opening time and a preparation method thereof. The invention provides a composite hot melt adhesive for an air filter material, which comprises the following components in parts by weight: 5-15 parts of polyisobutylene, 10-30 parts of metallocene catalyzed polypropylene, 20-70 parts of random polyolefin, 10-45 parts of petroleum resin and 0.1-1 part of antioxidant; the dosage ratio of the polyisobutylene to the random polyolefin is as follows: 1: (4-7), wherein the dosage of the polyisobutene is 6% -15% of the total dosage of the raw materials. The composite hot melt adhesive for the air filter material can prolong the opening time of products, so that the hot melt adhesive can be better compounded with other products for use.)

1. The composite hot melt adhesive for the air filter material is characterized by comprising the following components in parts by weight: 5-15 parts of polyisobutylene, 10-30 parts of metallocene catalyzed polypropylene, 20-70 parts of random polyolefin, 10-45 parts of petroleum resin and 0.1-1 part of antioxidant; the dosage ratio of the polyisobutylene to the random polyolefin is as follows: 1: (4-7), wherein the dosage of the polyisobutene is 6% -15% of the total dosage of the raw materials.

2. The composite hot melt adhesive for air filters as claimed in claim 1, wherein the amount of polyisobutylene is 8-15% of the total amount of raw materials.

3. The composite hot melt adhesive for air filters as claimed in claim 2, wherein the amount of polyisobutylene is 10-15% of the total amount of raw materials.

4. The composite hot melt adhesive for air filters as claimed in claim 3, wherein the amount of polyisobutylene is 12-15% of the total amount of raw materials.

5. The composite hot melt adhesive for air filters as claimed in claim 1, wherein the amount of the random polyolefin is 40-65% of the total amount of the raw materials.

6. The composite hot melt adhesive for air filters as claimed in claim 1, wherein the amount ratio of the polyisobutylene to the random polyolefin is: 1: (5-6).

7. The composite hot melt adhesive for air filters as claimed in claim 1, wherein the adhesive comprises 6 to 15 parts of polyisobutylene, 15 to 25 parts of metallocene-catalyzed polypropylene, 20 to 65 parts of random polyolefin, and 35 to 40 parts of petroleum resin.

8. The compound hot melt adhesive for air filters as claimed in claim 1, wherein the antioxidant is antioxidant 1010 and/or antioxidant 168.

9. The preparation method of the compound hot melt adhesive for the air filter material according to any one of claims 1 to 8, which is characterized by comprising the following steps:

(1) preheating a reaction kettle;

(2) adding polyisobutylene into a reaction kettle, heating to 170-230 ℃, stirring at the stirring speed of 20-50 revolutions per minute until the polyisobutylene is completely molten, and keeping the temperature at 170-230 ℃;

(3) sequentially adding metallocene polyolefin and random polyolefin, dissolving one by one, stirring at 20-50 r until the metallocene polyolefin and the random polyolefin are completely molten, and keeping the temperature at 170-230 ℃;

(4) adding petroleum resin and antioxidant in turn, and reducing stirring speed by 10-30 r. And (5) after fully and uniformly stirring, introducing into a screw extruder for extruding and granulating.

10. The preparation method of the compound hot melt adhesive for the air filter material according to claim 9, wherein in the step (2), the temperature is raised to 170-190 ℃ and the mixture is stirred; in the step (2) and the step (3), the temperature is kept at 170-190 ℃.

Technical Field

The invention belongs to the technical field of hot melt adhesives, and particularly relates to a composite hot melt adhesive for an air filter material and a preparation method thereof.

Background

The air filter is used as a device for protecting breathing, and with the increasing severity of environmental pollution and the increasing awareness of the environment, the air quality has become a global focus of attention, resulting in the increasingly widespread use of air filters. With the continuous development of the design of the filter itself, barrier-free filters have emerged, from which hot melt adhesives have found widespread use in filters. In the air filter without the partition plate, the hot melt adhesive is used for replacing the aluminum foil of the filter with the partition plate to separate the filter materials. The filter without the partition plate not only eliminates the damage of the partition plate to the filter medium, but also effectively increases the filtering area, improves the filtering efficiency, and simultaneously reduces the airflow resistance, thereby reducing the energy consumption. Different from hot melt adhesives used in industrial production, the hot melt adhesives applied to the air filter materials have slightly lower requirements on bonding strength but higher requirements on environmental protection. At present, all raw materials used for indoor air filtration are required to be environment-friendly materials, so that secondary pollution to the environment is avoided. And all finished products must pass some safety certifications of third parties to ensure that the finished products are harmless to human bodies and defective products can be recycled. Therefore, the hot melt adhesive used in the conventional daily bonding and industrial production is difficult to be used as the hot melt adhesive of the air filter material.

The hot melt adhesive used for the air filter at present is mainly EVA (ethylene vinyl acetate copolymer), and the EVE type hot melt adhesive mainly has the problems: 1. the EVA hot melt adhesive has poor thermal stability, and can decompose low molecular substances with certain odor during heating and use, so that the quality of the air filter is seriously influenced; 2. during the thermal decomposition, severe color changes are also caused, thereby affecting the appearance of the air filter; 3. the low temperature resistance is poor, and severe low temperature can cause the EVA to become brittle or the bonding strength to be rapidly reduced; 4. the bonding strength is relatively general, and the use requirement cannot be met in some occasions.

In the prior art, a hot melt adhesive developed to replace an EVE-type hot melt adhesive also exists, for example, patent publication No. CN106497454A discloses a polyolefin hot melt adhesive for an air filter, which comprises the following components in parts by mass: 30-60 parts of metallocene catalyzed polyethylene; 20-50 parts of hydrogenated petroleum resin; 5-30 parts of Fischer-Tropsch wax; 0.1-10 parts of polyethylene wax; 0.1 to 2 portions of antioxidant. The hot melt adhesive is characterized in that the high temperature resistance of the product is improved by means of the high crystallinity of the Fischer-Tropsch wax, but the brittleness of the hot melt adhesive product is poor due to the addition of the Fischer-Tropsch wax, the opening time is short, and the hot melt adhesive is difficult to apply to some construction processes which need long opening time. The existing products for replacing EVE hot melt adhesives inevitably need wax products to avoid the phenomenon that the surface of the hot melt adhesive is sticky.

Patent publication No. CN108219711A discloses a polypropylene hot melt adhesive for an air filter, and a preparation method and application thereof. The hot melt adhesive comprises the following components in percentage by mass: 15-45% of polypropylene polymer, 8-24% of POP polymer, 15-45% of petroleum resin, 3-12% of polyisobutylene, 8-23% of Fischer-Tropsch wax, 1-10% of ethylene butyl acrylate copolymer and 0.2-1% of antioxidant. The liquid polyisobutylene resin can be used for endowing the product with the advantages of no odor, long opening time and good flexibility. However, the solution still cannot avoid the use of wax products, and the open time of the solution still cannot be prolonged more.

In conclusion, the opening time of the hot melt adhesive in the prior art is generally 5-10 seconds, which can meet the application requirement of the conventional hot melt adhesive. Some improved hot melt adhesives have a difficulty in increasing the open time of the hot melt adhesive to over 25 seconds due to the inevitable presence of wax products. For the hot melt adhesive which needs to be compounded with other materials, too short opening time causes great technical obstruction for compounding other products with the hot melt adhesive, and great improvement of the compound hot melt adhesive is difficult to realize.

Disclosure of Invention

Aiming at the defects of the prior art, the invention provides a composite hot melt adhesive for an air filter material with longer opening time and a preparation method thereof.

The invention provides a composite hot melt adhesive for an air filter material, which comprises the following components in parts by weight: 5-15 parts of polyisobutylene, 10-30 parts of metallocene catalyzed polypropylene, 20-70 parts of random polyolefin, 10-45 parts of petroleum resin and 0.1-1 part of antioxidant; the dosage ratio of the polyisobutylene to the random polyolefin is as follows: 1: (4-7), wherein the dosage of the polyisobutene is 6% -15% of the total dosage of the raw materials.

Preferably, the amount of the polyisobutylene is 8% -15% of the total amount of the raw materials.

Preferably, the amount of the polyisobutylene is 10% -15% of the total amount of the raw materials.

Preferably, the amount of the polyisobutylene is 12% -15% of the total amount of the raw materials.

Preferably, the amount of the random polyolefin is 40% to 65% of the total amount of the raw materials.

Preferably, the polyisobutylene and the random polyolefin are used in a ratio of: 1: (5-6).

Preferably, the polyisobutylene is 6-15 parts, the metallocene catalyzed polypropylene is 15-25 parts, the atactic polyolefin is 20-65 parts, and the petroleum resin is 35-40 parts.

Preferably, the antioxidant is antioxidant 1010 and/or antioxidant 168.

The invention also provides a preparation method of the compound hot melt adhesive for the air filter material, which comprises the following steps:

(1) preheating a reaction kettle;

(2) adding polyisobutylene into a reaction kettle, heating to 170-230 ℃, stirring at the stirring speed of 20-50 revolutions per minute until the polyisobutylene is completely molten, and keeping the temperature at 170-230 ℃;

(3) sequentially adding metallocene polyolefin and random polyolefin, dissolving one by one, stirring at 20-50 r until the metallocene polyolefin and the random polyolefin are completely molten, and keeping the temperature at 170-230 ℃;

(4) adding petroleum resin and antioxidant in turn, and reducing stirring speed by 10-30 r. And (5) after fully and uniformly stirring, introducing into a screw extruder for extruding and granulating.

Preferably, in the step (2), the temperature is increased to 170-190 ℃ and stirring is carried out; in the step (2) and the step (3), the temperature is kept at 170-190 ℃.

The composite hot melt adhesive for the air filter material can prolong the opening time of products, so that the hot melt adhesive can be better compounded with other products for use.

The composite hot melt adhesive for the air filter material provided by the invention can realize the opening time of 1-5 minutes, so that the hot melt adhesive can be better compounded with other materials in the using process, the variety of the hot melt adhesive composite material is widened, and the excellent performance of the filter material product is realized.

Detailed Description

The technical solutions of the present invention are further described in detail with reference to specific examples so that those skilled in the art can better understand the present invention and can implement the present invention, but the examples are not intended to limit the present invention.

The embodiment of the invention provides a composite hot melt adhesive for an air filter material, which comprises the following components in parts by weight: 5-15 parts of polyisobutylene, 10-30 parts of metallocene catalyzed polypropylene, 20-70 parts of random polyolefin, 10-45 parts of petroleum resin and 0.1-1 part of antioxidant; the dosage ratio of the polyisobutylene to the random polyolefin is as follows: 1: (4-7), wherein the dosage of the polyisobutene is 6-15% of the total dosage of the raw materials.

In the embodiment, the polyisobutylene is used as a viscosity and open time regulator, so that the good fluidity and dispersibility of the hot melt adhesive are realized. The polyisobutylene is used as a flexibilizer, so that the polyolefin can obtain better flexibility, the opening time is prolonged, the random polyolefin has good surface wetting and spreading performance and better compatibility with resins, and the petroleum resin is used as a tackifier, so that the bonding performance of the product is effectively improved. A small amount of antioxidant can relieve the aging of the material in the heating process and prolong the service life of the finished product in daily use.

In the embodiment, the wax material is omitted, and the polyisobutylene is selected as the viscosity and open time regulator, wherein the dosage of the polyisobutylene is 6-15% of the total dosage of the raw materials, so that the open time of the hot melt adhesive is longer and can reach 1-5 minutes. In the embodiment, random polyolefin is selected, the internal space of the random polyolefin is relatively large, the dosage ratio of the random polyolefin to polyisobutylene is limited, the random polyolefin and the polyisobutylene can be well matched, the polyisobutylene can be well fused in the random polyolefin, and the sticky phenomenon of the hot melt adhesive caused by more polyisobutylene is avoided.

In a preferred embodiment, the random polyolefin is a random polyalphaolefin.

In a preferred embodiment, the amount of polyisobutene used is from 8% to 15% of the total amount of starting materials. In a further preferred embodiment, the polyisobutene is used in an amount of from 10% to 15% of the total amount of starting materials. In a further preferred embodiment, the amount of polyisobutene is from 12% to 15% of the total amount of starting materials. The higher polyisobutylene ensures the flexibility of the hot melt adhesive and prolongs the opening time of the hot melt adhesive.

In a preferred embodiment, the amount of random polyolefin is 40% to 65% of the total amount of the feedstock. The use of a larger amount of the random polyolefin can avoid the stickiness caused by the use of a larger amount of the polyisobutylene.

In a preferred embodiment, the polyisobutylene and random polyolefin are used in a ratio of: 1: (5-6).

In a preferred embodiment, the composite material comprises 6-15 parts of polyisobutylene, 15-25 parts of metallocene-catalyzed polypropylene, 20-65 parts of random polyolefin and 35-40 parts of petroleum resin.

In a preferred embodiment, the antioxidant is antioxidant 1010 and/or antioxidant 168.

The embodiment of the invention also provides a preparation method of the compound hot melt adhesive for the air filter material, which comprises the following steps:

(1) preheating a reaction kettle;

(2) adding polyisobutylene into a reaction kettle, heating to 170-230 ℃, stirring at the stirring speed of 20-50 revolutions per minute until the polyisobutylene is completely molten, and keeping the temperature at 170-230 ℃;

(3) sequentially adding metallocene polyolefin and random polyolefin, dissolving one by one, stirring at 20-50 r until the metallocene polyolefin and the random polyolefin are completely molten, and keeping the temperature at 170-230 ℃;

(4) adding petroleum resin and antioxidant in turn, and reducing stirring speed by 10-30 r. And (5) after fully and uniformly stirring, introducing into a screw extruder for extruding and granulating.

In a preferred embodiment, in the step (2), the temperature is raised to 170-190 ℃ and stirring is carried out; and (3) keeping the temperature at 170-190 ℃.

In order that the technical solutions of the present invention may be further understood and appreciated, several preferred embodiments are now described in detail.

The specifications of the raw materials used in the examples of the present invention are shown in table 1.

TABLE 1

Specific formulations of the inventive examples and comparative examples are shown in table 2.

TABLE 2

The preparation methods of examples 1 to 3 and comparative examples 1 to 3 were as follows:

(1) and preheating the reaction kettle.

(2) Adding polyisobutylene, or polyisobutylene and polypropylene wax, or polypropylene wax into a reaction kettle, heating to 180 ℃, stirring at the stirring speed of 20-50 rpm until the polyisobutylene, or polyisobutylene and polypropylene wax, or polypropylene wax are completely melted and kept at a constant temperature.

(3) The metallocene polyolefin and the random polyolefin are added according to the viscosity from low to high, and are dissolved one by one, the stirring speed is 20-50 revolutions, and the mixture is completely melted and kept at the constant temperature of 180 ℃.

(4) Adding petroleum resin and antioxidant in turn, and reducing stirring speed by 10-30 r. And (5) after fully and uniformly stirring, introducing into a screw extruder for extruding and granulating.

The preparation method of comparative example 4 was:

heating the mixer to 150 ℃, putting the polyisobutylene and the butyl rubber into the mixer, and mixing for 20 minutes; filling nitrogen into a reaction kettle, putting the mixed polyisobutylene and butyl rubber mixture, amorphous polyolefin, metallocene polypropylene, petroleum resin and anti-aging agent into the reaction kettle, heating at 150 ℃, and stirring at the speed of 150 revolutions per minute; stopping heating the reaction kettle when the mixture in the reaction kettle is in a molten state, pressurizing and discharging, wherein the pressure in the reaction kettle is 0.2MPa, and filtering a finished product by using a 150-mesh filter screen during discharging; and (5) making a fixed model by using white glassine paper, containing the discharged finished product, and packaging and warehousing after the finished product is cooled.

And (3) performance measurement:

the hot melt adhesive provided by examples 1-3 and comparative examples 1-4 of the present invention was tested for its relevant properties by the following methods:

(1) the softening point and the melt viscosity are detected according to the related item detection method of HG/T3698-2002 EVA hot-melt adhesive.

(2) And the curing time means that the glue is melted and then scraped on a paper board, then the other paper board is attached, timing is carried out from the completion of the attachment, peeling is carried out from one end until the base material is cut to be broken, namely the glue is cured, and the recorded time is the curing time of the glue.

(3) The thermal stability test is to melt 100g of the glue sample at 160 ℃ and keep the glue sample at 160 ℃ for 4 hours, then observe whether the color of the glue is obviously changed, if so, judge the glue sample to be unstable.

(4) Hazardous substance test conditions: the 211 high interest Substances (SVHC) were subjected to screening tests based on the candidate list of high interest substances for authorization consultation published by the european chemical administration by 2021, month 1, 19 (according to REACH regulation No. 1907/2006 of the european union). The test results for the high concern Substance (SVHC) in the sample satisfied ≦ 0.1% (w/w) passed, otherwise failed.

Specific test results are shown in table 3.

TABLE 3

The data in table 1 show that the hot melt adhesive products prepared in the embodiments 1 to 3 have a long curing time, can well prolong the open time, and have an open time of more than 3 minutes, and the effect is very significant. The melt viscosities measured in examples 1-3 were 3000. + -. 500CPS/180 ℃ and no stickiness occurred during the use of the hot melt adhesive.

In comparative example 1, the open time of the product was adjusted by using polypropylene wax instead of polyisobutylene, and no stickiness occurred during the use of the hot melt adhesive, but the open time of the obtained hot melt adhesive was short, only 5-7s, and thus, it can be seen that the effect of the extended open time of examples 1-3 was very significant.

In comparative example 2, polyisobutylene and polypropylene wax are mixed to avoid the stickiness phenomenon in the use process of the hot melt adhesive, but because the polyisobutylene is used in a small amount, the effect of prolonging the opening time cannot be achieved well, and the opening time of the product cannot be improved obviously.

In comparative example 3, the polyisobutylene is used for adjusting the opening time of the product, the opening time is prolonged remarkably, but because the polyisobutylene is used in a large amount and the proportion of the polyisobutylene and the random polyolefin is not reasonable, the obtained hot melt adhesive is seriously sticky in the using process and is difficult to apply.

In comparative example 4, the combination of polyisobutylene and random polyolefin is adopted, although the opening time of the hot melt adhesive product can be prolonged to a certain extent, the hot melt adhesive is not a product applied to the air filter material, is mainly applied to the fields of diaper and pull-up diaper, has different specific formulas from examples 1 to 3, and cannot be used as the hot melt adhesive used in the field of the air filter material because the test of harmful substances fails. And although the opening time of the hot melt adhesive product can be prolonged, the opening time of the hot melt adhesive product is still not significant because the other component proportions are different from those of the hot melt adhesive products of the embodiments 1 to 3. Therefore, it can be seen that the hot melt adhesive field has been developed for many years and has good application in various fields, but the application of the common industrial hot melt adhesive in the air filter material field cannot meet the environmental protection requirement. Therefore, the hot melt adhesive formula in the field of air filter materials also has a mature system, and can not be realized simply according to common industrial hot melt adhesives.

In conclusion, the hot melt adhesive applied to the air filter material can remarkably prolong the opening time of the hot melt adhesive, ensure that the hot melt adhesive is not sticky in the using process, better apply the hot melt adhesive and widen the using process, and realize that the hot melt adhesive applied to the air filter material can accord with other materials to improve the hardness.

The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.