Maleic anhydride grafted linear low-density polyethylene adhesive resin and preparation method thereof

A linear low-density, maleic anhydride technology, applied in the field of polymer materials, can solve the problems of difficult sublimation of maleic anhydride, less residual monomers, and low surface energy, and achieve less residual monomers, simple reaction process, and improved Effect of Adhesive Strength

Pending Publication Date: 2021-12-07
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

[0005] The present invention aims to solve the problem of low surface energy of the existing polyethylene film, prepare a high-grafting ...
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Method used

Table 1 is the test data of the product prepared by embodiment 1-3. It can be seen from Table 1 that the graft copolymer LLDPE-g-MAH synthesized by melt grafting method in the kettle shows that the adjusted grafting process improves the grafting rate of the common method. The peel strength of the polyethylene composite film increases with the increase of the grafting ratio of LLDPE-g-MAH adhesive resin, the peel strength increases from 4.6N to 12N, and ...
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Abstract

The invention discloses maleic anhydride grafted linear low-density polyethylene adhesive resin and a preparation method thereof. The adhesive resin is prepared from the following components in parts by weight: 100 to 120 parts of solvent, 80 to 100 parts of linear low-density polyethylene, 0.05 to 0.5 part of maleic anhydride, 0.01 to 0.1 part of peroxide initiator and 0 to 1.5 parts of comonomer. The adhesive resin is prepared by the following steps: (1) weighing the solvent, polyethylene and maleic anhydride according to the ratio, heating and stirring, dissolving, and evaporating out the solvent; (2) controlling the temperature to be 100-150 DEG C, introducing N2, and adding the initiator in five times; raising the temperature to 150-200 DEG C, keeping the temperature for 3 hours, washing and drying; and (3) heating and dissolving the crude product in a solvent, cooling, pouring into the solvent, standing, carrying out suction filtration, and drying to obtain a grafted product. The problems of poor mixing effect, multiple side reactions and the like of screw processing can be effectively solved, and the grafting rate of grafted resin is increased. The material can be used as resin with large bonding polarity difference or used as a high-molecular compatilizer.

Technology Topic

Maleic anhydrideSolvent +8

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  • Maleic anhydride grafted linear low-density polyethylene adhesive resin and preparation method thereof

Examples

  • Experimental program(3)

Example Embodiment

[0021] Example 1
[0022] Maleic anhydride grafted linear low density polyethylene adhesive resin and preparation method. Parts by weight: 110 parts of a solvent, 100 parts of linear low density polyethylene, 1 part of maleic anhydride, 2 parts of peroxide initiators, comonomers 0 parts. Said solvent is acetone. The linear low density polyethylene of melt index of 1g / 10min. The maleic anhydride is maleic anhydride monomers. The peroxide-based initiator is benzoyl peroxide.
[0023] Maleic anhydride grafted linear low density polyethylene adhesive resins, characterized by comprising the steps of:
[0024] Step 1: The solvent, linear low density polyethylene and maleic anhydride in the above ratio were weighed, mixed and stirred in a four-necked flask, maintained at a temperature of 50 ℃, warmed until both fully dissolved and the solvent was distilled off.
[0025] Step 2: controlling the temperature of 105 ℃, heating while stirring into N 2 , In an oxygen-free state within the holding tank, and then the initiator is slowly added in 5 minutes, avoid oxidative decomposition, after continued stirring for controlling temperature; the reaction temperature was raised to 160 ℃ reaction temperature and held 3h, washed and dried to give impurity-containing graft polymer synthesis.
[0026] Step 3: The step 2 The crude product obtained is added a solvent, was heated at reflux for 1h and open the condensate, after the mixture was cooled poured into a solvent, allowed to stand suction filtration, and drying to obtain a graft product was purified.

Example Embodiment

[0027] Example 2
[0028] Maleic anhydride grafted linear low density polyethylene adhesive resin and preparation method. Parts by weight: 110 parts of a solvent, 100 parts of linear low density polyethylene, 6 parts of maleic anhydride, 2 parts of peroxide initiators, comonomers 0 parts. Said solvent is acetone. The linear low density polyethylene of melt index of 1g / 10min. The maleic anhydride is maleic anhydride monomers. The peroxide-based initiator is benzoyl peroxide.
[0029] Maleic anhydride grafted linear low density polyethylene adhesive resins, characterized by comprising the steps of:
[0030] Step 1: The solvent, linear low density polyethylene and maleic anhydride in the above ratio were weighed, mixed and stirred in a four-necked flask, maintained at a temperature of 50 ℃, warmed until both fully dissolved and the solvent was distilled off.
[0031] Step 2: controlling the temperature of 105 ℃, heating while stirring into N 2 , In an oxygen-free state within the holding tank, and then the initiator is slowly added in 5 minutes, avoid oxidative decomposition, after continued stirring for controlling temperature; the reaction temperature was raised to 160 ℃ reaction temperature and held 3h, washed and dried to give impurity-containing graft polymer synthesis.
[0032] Step 3: The step 2 The crude product obtained is added a solvent, was heated at reflux for 1h and open the condensate, after the mixture was cooled poured into a solvent, allowed to stand suction filtration, and drying to obtain a graft product was purified.

Example Embodiment

[0033] Example 3
[0034] Maleic anhydride grafted linear low density polyethylene adhesive resin and preparation method. Parts by weight: 110 parts of a solvent, 100 parts of linear low density polyethylene, 12 parts of maleic anhydride, 2 parts of peroxide initiators, comonomers 0 parts. Said solvent is acetone. The linear low density polyethylene of melt index of 1g / 10min. The maleic anhydride is maleic anhydride monomers. The peroxide-based initiator is benzoyl peroxide.
[0035] Maleic anhydride grafted linear low density polyethylene adhesive resins, characterized by comprising the steps of:
[0036] Step 1: The solvent, linear low density polyethylene and maleic anhydride in the above ratio were weighed, mixed and stirred in a four-necked flask, maintained at a temperature of 50 ℃, warmed until both fully dissolved and the solvent was distilled off.
[0037] Step 2: controlling the temperature of 105 ℃, heating while stirring into N 2 , In an oxygen-free state within the holding tank, and then the initiator is slowly added in 5 minutes, avoid oxidative decomposition, after continued stirring for controlling temperature; the reaction temperature was raised to 160 ℃ reaction temperature and held 3h, washed and dried to give impurity-containing graft polymer synthesis.
[0038] Step 3: The step 2 The crude product obtained is added a solvent, was heated at reflux for 1h and open the condensate, after the mixture was cooled poured into a solvent, allowed to stand suction filtration, and drying to obtain a graft product was purified.
[0039] Graft resin film varying amounts of samples to detect the effect of graft resin adhesive peel strength test. JY-HB-021 by a small electronic tensile testing machine, controlling the stretching rate v = 50mm / min, each test sample comprising a 5 spline, each spline is 10cm long, 15mm wide, each strip taking test samples as a final test average value.
[0040] Using known graft ratio of LLDPE-g-MAH graft resin infrared established standard curve fitting and wherein the graft ratio of infrared peak intensity ratio of the equation to measure the graft ratio of the graft resin.
[0041] MAH grafting rate equation:
[0042]
[0043] Where: GD-maleic anhydride grafting rate (%);
[0044] A 1715 - 1715cm corresponding to the grafted resin infrared spectrum -1 The peak of the office;
[0045] A 1380 - 1380cm corresponding to the grafting resin infrared spectrum -1 Peak
[0046] Table 1 is a test data for the product prepared by Example 1-3. From Table 1, it is possible to see the molten graft method in the kettle, the synthetic graft copolymer LLDPE-G-MAH, indicating that the adjusted graft process increases the graft rate of the common method. The peel strength of the polyethylene composite film increases with the increase of LLDPE-G-MAH bonding resin, the peel strength is getting larger, and the peeling force is increased from 4.6 N to 12 N, and the bonding effect is getting better and better. This is due to the increase of the adhesive resin content, the number of maleic anhydride polar groups also increases, increasing the polarity of the polyethylene matrix, and the interface tension of the two phases of the polarity material is reduced, while LLDPE-G -Mah bonding resin is copolymerized with polar material, and also enhances the bonding effect of both.
[0047] Table 1 Test data of the product prepared by Example 1-3
[0048] Example 1 2 3 Grafting rate (%) 0.5 3.5 8.3 Peeling force (N) 4.6 6.4 12.0

PUM

PropertyMeasurementUnit
Melt index1.0g/10min

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