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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, difficult to find solvents, complicated processing procedures, etc., and achieves long preparation cycle, low price, and satisfactory Effects of performance requirements

Inactive Publication Date: 2006-09-20
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
Comparison scheme
Effect test

Embodiment 1

[0057] Mix organoclay (organosodium-based bentonite) and oleic acid in a mass ratio of 1:1, stir on a mixer for 30 minutes to obtain pre-expanded organoclay, and mill 100 parts of butyl rubber and 5 parts of pre-expanded organoclay in a double-roller Mix on the machine for about 30 minutes, then add the following ingredients in three steps, the first step is to add 5 parts of zinc oxide, 2 parts of stearic acid, and the second step is to add 2-mercaptobenzothiazole (accelerator M) 0.5 parts, 1.0 parts of tetramethylthiuram disulfide (accelerator TMTD), 1.0 parts of N-phenyl-α-naphthylamine (anti-aging agent A), 1.8 parts of sulfur are added in the third step, and after mixing for 20 minutes The rubber material is rolled down to obtain the nano-composite material of butyl rubber and clay. Then measure its positive vulcanization time (T90) at 160°C, vulcanize on a flat vulcanizing machine according to the positive vulcanization time, and prepare samples. Transmission electron m...

Embodiment 2

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

Embodiment 3

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

[0064]As can be seen from Table 1, the butyl rubber / clay nanocomposite prepared by the pre-expanded organoclay processed with n-butanol in the present invention has hardness, 100% modulus, 300% modulus, and tensil...

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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 method for preparing a rubber-clay nanocomposite material, in particular to a method for preparing the clay-rubber nanocomposite 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. The most commonly used of these is montmorillonite, also known as bentonite. However, as a filler, inorganic clay has poor reinforcing ability, so it can only be used in traditional microcomposites. Montmorillonite has a lamellar structure, and some ions between layers can be exchanged with other organic ions. Organoclay is obtained by modifying inorganic clay. Such as the use of cetyl ammonium bromide prepared by ion exchange reaction. The preparation method of organic montmorillonite was reported in "EPDM / montmorillo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/40C08L9/02
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