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A kind of reprocessable elastomer and its preparation method

A technology for repeated processing and elastomers, applied in the field of elastomers, can solve problems such as poor selectivity, uneven distribution between polar group chains, and difficult removal of residual reactants, so as to reduce reaction costs, shorten overall time, and simplify reactions. The effect of steps

Active Publication Date: 2022-06-17
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reversible chemical crosslinking groups of the above-mentioned reproducible elastomers are generally completed by adding polar functional groups to the existing polymers through post-reaction, and the cis-1,4 regular chain structure of rubber molecules is destroyed, resulting in poor selectivity and side reactions. Many, residual reactants are difficult to remove, unsuitable for large-scale application, etc.
In addition, the location, number and reactivity of reactive sites are often difficult to control when adding polar groups at a later stage, and the rubber network topology is difficult to control, which create difficulties in the production and post-processing and performance of reproducible elastomers
For example, in common butadiene rubber, the number and position of natural rubber functional groups are difficult to determine, and the content of cis-1,4 is reduced. Branch modification, the operation is generally complicated and cumbersome, and the reaction sites cannot be precisely controlled. At the same time, the distribution of polar groups between chains is uneven, making the reversible crosslinking network structure uneven.

Method used

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  • A kind of reprocessable elastomer and its preparation method
  • A kind of reprocessable elastomer and its preparation method
  • A kind of reprocessable elastomer and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] (1) Synthesis of epoxy myrcene: First, completely dissolve myrcene in 20 times the volume of dichloromethane, freeze at 0°C for 2 hours, and slowly add m-chloroperoxybenzoic acid (m -CPBA), return to room temperature, monitor the reaction by TLC until the reaction of the raw materials is complete, add 2M NaOH aqueous solution to neutralize the excess acid, wash with water and retain the organic phase, use anhydrous magnesium sulfate to dry the organic phase, filter under reduced pressure distillation, column Chromatographic separation and purification to obtain a colorless transparent liquid is epoxy myrcene;

[0082] Epoxymyrcene: 1 H NMR (400MHz, CDCl 3 ): 6.38(dd,1H,J=17.6,10.8Hz,),5.27(d,1H,J=17.6Hz),5.07(dd,3H,J=16.6,9.2Hz),2.76(t,1H,J =6.3Hz),2.44(dd,1H,J=14.9,7.7Hz),2.32(dt,1H,J=15.5,7.9Hz),1.77-1.73(m,2H),1.31(s,3H),1.26 (s, 3H);

[0083] 13 C NMR (100MHz, CDCl 3 ): 145.5, 138.6, 116.1, 113.4, 64.1, 58.4, 28.1, 27.6, 24.9, 18.8;

[0084] (2) Preparation o...

Embodiment 2

[0090] (1) the synthesis of epoxy myrcene: with embodiment 1;

[0091] (2) Preparation of aldehyde-based myrcene (formula 8): Ozone (1 atm) oxidized myrcene (1 mol) in methanol solution at room temperature, the reaction was terminated after 10 hours, methanol was spin-dried, dichloromethane was dissolved, saturated aqueous sodium bicarbonate solution Extraction, dewatering with anhydrous magnesium sulfate overnight, depressurizing distillation and purifying the monomer to obtain aldehyde myrcene with a yield of 94.1%;

[0092] Aldehydryl myrcene: 1 H NMR (400MHz, CDCl 3 ): 9.72(d, 1H), 6.32(m, 1H), 5.24(m, 1H), 5.05(m, 3H), 2.44(dt, 2H), 2.29(t, 2H);

[0093](3) Preparation of aldehyde-based myrcene modified isoprene rubber: using the ratio of isoprene: aldehyde-based myrcene molar amount=0.8:0.2, in an anhydrous and oxygen-free system, 272.7 mmol of aldehyde-based myrcene was added In a polymerization bottle containing 150 mL of n-hexane, 1087.3 mmol of isoprene and 272.7 ...

Embodiment 3

[0097] (1) the synthesis of epoxy myrcene: with embodiment 1;

[0098] (2) preparation of aldehyde group myrcene (formula 8): with embodiment 2;

[0099] (3) Preparation of aldehyde-based myrcene-modified isoprene rubber: using the ratio of isoprene: aldehyde-based myrcene molar amount=0.95:0.05, in an anhydrous and oxygen-free system, 68.9 mmol of aldehyde-based myrcene was added to the In a polymerization bottle containing 100 mL of n-hexane, 1291.1 mmol of isoprene and 68.9 mmol of triisobutylaluminum were successively added, stirred for half an hour to shield the aldehyde group, and 0.20 mmol of neodymium (III) neocaprate was added. Then 28.9 mmol of triisobutylaluminum and 0.40 mmol of diethylaluminum chloride were added to initiate polymerization, and the whole process was nitrogen atmosphere, and the temperature of the reaction system was kept at 30 ° C; The methanol solution was precipitated and washed, filtered and dried to obtain a clean copolymer with a yield of 87...

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Abstract

The invention discloses a reprocessable elastic body, which is characterized in that, in terms of mole fractions, it comprises the following raw materials: 0.1 to 2 parts of conjugated diene polar monomers containing functional groups, non-polar copolymer monomers 8-10 parts of body, 0.1-2 parts of shielding agent, 0.00001-0.0001 parts of polymerization catalyst, 25-75 parts of solvent B, 0.1-2.5 parts of crosslinking agent; by mole parts, conjugated diene polar monomers include The following raw materials: 5-8.5 parts of Lewis base, 40-80 parts of solvent A, 5-7.5 parts of compounds containing functional groups, 5-5.5 parts of epoxy myrcene, 5-7.5 parts of dehydration catalysts; functional groups are epoxy, At least one of pyridine, furan, aldehyde group and ester group. The invention also discloses a preparation method of the above-mentioned reproducible elastic body. The reprocessable elastomer of the present invention has a reversible cross-linking structure, controllable cross-linking points, and high cis-1,4 content.

Description

technical field [0001] The invention relates to the technical field of elastomers, in particular to a reprocessable elastomer and a preparation method thereof. Background technique [0002] Traditional rubber usually uses sulfur vulcanization or peroxide vulcanization to form irreversible chemical cross-linking bonds, which has high stability. The waste of rubber products leads to a lot of waste of petroleum resources and environmental pollution, which is not conducive to sustainable development; on the other hand, a large amount of sulfur compounds are generated during the rubber vulcanization and cross-linking process, which leads to serious environmental problems in the plant area and the environment. , or the peroxy compound has poor stability and is prone to explosion during operation. [0003] At present, it has been reported that by epoxidizing the rubber matrix and adding reversible covalent crosslinking agents such as dicarboxylic acids, the repeatable processing a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F236/08C08F236/22C08F236/14C08J3/24C07D303/22C07D213/70C07C45/40C07C47/21C07D307/38C07C319/14C07C323/52C08L9/00
CPCC08F236/08C08J3/24C07D303/22C07D213/70C07C45/40C07D307/38C07C319/14C08J2309/00C08F236/22C08F236/14C07C47/21C07C323/52
Inventor 龚狄荣胡中瀚徐月超罗琬惟黄炜众
Owner NINGBO UNIV