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Process for preparing rubber and clay nano composites by using pre-expanded organic clay

A nanocomposite material and organoclay technology, which is applied in the field of preparation of rubber and clay nanocomposite materials, can solve the problems of inability to prepare butyl rubber, complicated processing procedures, difficulty in finding solvents, etc., achieves long preparation cycle, meets performance requirements, Inexpensive effect

Inactive Publication Date: 2005-09-14
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Although the solution intercalation method can simplify the process (compared with in-situ polymerization), it is difficult to find a solvent that can dissolve the polymer and disperse the montmorillonite on the one hand, and use a large amount of organic solvents on the other hand. Harmful to the human body and pollute the environment
The third aspect is that the solution intercalation method not only uses an organic solvent to disperse the clay, so that the clay can be pre-expanded, but also uses an organic solvent to dissolve the rubber, and then a large amount of organic solvent needs to be volatilized and removed during the process. Generally, it takes 5 to volatilize. Days, so the whole process is more complicated and time-consuming
[0018] The emulsion polymerization method mainly utilizes the advantage that most rubbers have their own emulsion form, the process is the simplest, easy to control, and the cost is the lowest, but the disadvantage is that when the mass fraction of clay is high (greater than 20%), the dispersibility is not as good as The in-situ intercalation method is good. In addition, for butyl rubber that has no emulsion at present, the emulsion polymerization method cannot be used to prepare butyl rubber / clay nanocomposites.

Method used

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  • Process for preparing rubber and clay nano composites by using pre-expanded organic clay
  • Process for preparing rubber and clay nano composites by using pre-expanded organic clay
  • Process for preparing rubber and clay nano composites by using pre-expanded organic clay

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Organoclay (organic sodium bentonite) was mixed with oleic acid in a mass ratio of 1:1, stirred on a mixer for 30 minutes to obtain pre-expanded organoclay, and 100 parts of butyl rubber and 5 parts of pre-expanded organoclay were smelted on two rolls. Mixing on the machine for about 30 minutes, then add the following various ingredients in three steps, the first step adds 5 parts of zinc oxide, 2 parts of stearic acid, the second step adds 2-thiol benzothiazole (accelerator M) 0.5 part, 1.0 part of tetramethylthiuram disulfide (accelerator TMTD), 1.0 part of N-phenyl-α-naphthylamine (anti-aging agent A), 1.8 part of sulfur was added in the third step, after mixing for 20 minutes The rubber material is rolled down to obtain a butyl rubber and clay nanocomposite material. Then measure its positive vulcanization time (T 90 ), vulcanized on a flat vulcanizer according to the positive vulcanization time, and prepared samples. Transmission electron microscopy (TEM) picture...

Embodiment 2

[0061] The organic solvent was changed to toluene, and the remaining operation steps were the same as those in Example 1 to obtain butyl rubber / clay nanocomposite. The mechanical properties of the materials are listed in Table 1, transmission electron microscopy pictures TEM (such as figure 2 shown), X-ray diffraction pattern (XRD) (e.g. Image 6 shown). from figure 2 It can be seen from the TEM photo of the pre-expanded organoclay treated with toluene that the dispersion structure of the prepared nanocomposites is finer, indicating that the organoclay has good dispersibility in toluene, which is conducive to the insertion of rubber macromolecular chains. It is an intercalated butyl rubber / clay nanocomposite. Image 6 The interlayer spacing of the pre-expanded organoclay corresponding to curve 1 increases from 4.2 nm to 5.1 nm, and the peak value of the nanocomposite corresponding to curve 2 is 6.5 nm, indicating that the rubber macromolecular chain is well inserted betwe...

Embodiment 3

[0063] The organic solvent was changed to n-butanol, and the remaining operation steps were the same as those in Example 1 to obtain butyl rubber / clay nanocomposite. The mechanical properties of the materials are listed in Table 1, and the transmission electron microscope photographs TEM are as follows. image 3 , the X-ray diffraction pattern (XRD) is shown as Figure 7 shown. from image 3 It can be seen from the TEM photo of the butyl rubber / clay nanocomposites prepared with n-butanol-treated pre-expanded organoclay that the dispersed phase structure is an exfoliated structure, indicating that the organoclay has been exfoliated into a single layer in n-butanol. . Thus, pre-expanded organoclay treated with n-butanol results in exfoliated nanocomposites.

[0064] As can be seen from Table 1, the butyl rubber / clay nanocomposite prepared by the pre-expanded organoclay treated with n-butanol in the present invention has the hardness, 100% constant elongation stress, 300% const...

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Abstract

This invention is a method of preparing rubber and clay nanometer compound material with pre-expand organic clay. Pre-expand organic clay is got by quality ratio 1:1 of organic solution and organic clay. Rubber and clay nanometer compound material is got by pre-expand organic clay and rubber and addition agent mixing. The organic solvents are toluene, oleic acid, castor oil or normal butyl alcohol. 3~7 quality portions of pre-expand organic clay is added into 100 portions rubber. The organic solvent dosage is few, and organic solvent that does no harm to human body and environment can be used. The operation method is simple, and easy to industrial generation.

Description

technical field [0001] The invention relates to a preparation method of rubber and clay nano-composite material, in particular to a method for preparing clay and rubber nano-composite material by blending pre-expanded organic clay and rubber. Background technique [0002] Clay is an abundant and inexpensive natural material that has long been used as a filler in the rubber industry. Such as kaolin, montmorillonite, red clay and clay and other series of fillers. One of the most commonly used is montmorillonite, also known as bentonite. However, inorganic clays have poor reinforcing ability as fillers, so they can only be used in traditional micro-composites. Montmorillonite has a lamellar structure, and some ions between layers can be exchanged with other organic ions. Organoclay is obtained by modifying inorganic clays. For example, it is prepared by ion exchange reaction using cetyl ammonium bromide. In "EPDM / Montmorillonite Nanocomposite I Preparation, Characterization...

Claims

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Application Information

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IPC IPC(8): C08L9/02C08K5/40
Inventor 张立群梁玉蓉吴友平徐燕莉张惠峰王益庆
Owner BEIJING UNIV OF CHEM TECH
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