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Preparation method of adhesive purpose chloroprene rubber

A neoprene and bonding technology, which is applied in the field of preparation of adhesive neoprene rubber, can solve the problem of unstable solubility of adhesive neoprene rubber, large deviation of Mooney viscosity and other performance indicators, and no re-initiation single problem

Inactive Publication Date: 2011-05-25
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 3. The polymer has no active end, and the active chain free radical will terminate its activity after chain transfer, and has no ability to re-initiate the monomer;
[0007] 4. Adhesive chloroprene rubber produced in different batches with the same formula has unstable solubility and large deviations in Mooney viscosity and other performance indicators

Method used

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  • Preparation method of adhesive purpose chloroprene rubber
  • Preparation method of adhesive purpose chloroprene rubber
  • Preparation method of adhesive purpose chloroprene rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1.05g of iodoform (accounting for 0.15% of monomer mass) and 25.00g of disproportionated rosin were uniformly dissolved in 700g of chloroprene monomer (CP), and the oil phase preparation temperature was 15°C±2°C. The configured oil phase was added to a 2000ml four-necked bottle, and the water phase (900g water, 1.40g sodium carbonate, 1.40g sodium lauryl sulfate, 0.85gLOMAR PW, 2.50g sodium hydroxide) was added under stirring. Claims no emulsification for 35 minutes at °C. Then cool down, add a redox initiator composed of 1.35g potassium persulfate, 1.85g sodium sulfite and 0.70g sodium formamidine sulfinate, and carry out polymerization reaction at 5°C-10°C. When the chloroprene conversion rate reaches 91%, add the terminator phenothiazine once under stirring, stir for 20 minutes to terminate the polymerization reaction, then adjust the pH value to 5-6 with acetic acid, and then use 3 liters of saturated CaCl 2 Solution gel, after washing with water on the rubber mixe...

Embodiment 2

[0029] 1.44g of iodoform (accounting for 0.205% of monomer mass) and 22.50g of disproportionated rosin were uniformly dissolved in 700g of chloroprene monomer (CP), and the oil phase preparation temperature was 15°C±2°C. The configured oil phase was added to a 2000ml four-necked bottle, and the water phase (900g water, 1.40g sodium carbonate, 1.40g sodium lauryl sulfate, 1.85g LOMAR PW, 3.05g sodium hydroxide) was added under stirring. Emulsify at ℃ for 35 minutes. Then cool down, add a redox initiator composed of 1.80g potassium persulfate, 2.10g sodium sulfite and 1.50g sodium formamidine sulfinate, and carry out polymerization reaction at 5°C-10°C. When the conversion rate of chloroprene reaches 94%, add the terminator phenothiazine once under stirring, stir for 20 minutes to terminate the polymerization reaction, then adjust the pH value to 5-6 with acetic acid, and then use 3 liters of saturated CaCl 2 The solution gel was washed with water on the rubber mixer and dried ...

Embodiment 3

[0031] 1.54g of iodoform (accounting for 0.22% of monomer mass) and 25.00g of disproportionated rosin were uniformly dissolved in 700g of chloroprene monomer (CP), and the oil phase preparation temperature was 15°C±2°C. Add the configured oil phase into a 2000ml four-necked bottle, add the water phase (900g water, 1.40g sodium carbonate, 1.40g sodium lauryl sulfate, 0.85gLOMAR PW, 2.50g sodium hydroxide) under stirring, Emulsify at ℃ for 25 minutes. Then cool down, add a redox initiator composed of 1.35g potassium persulfate, 1.85g sodium sulfite and 0.70g sodium formamidine sulfinate, and carry out polymerization reaction at 5°C-10°C. When the chloroprene conversion rate reaches 93%, add the terminator phenothiazine once under stirring, stir for 25 minutes to terminate the polymerization reaction, then use 3 acetic acid to adjust the pH value to 5-6, and then use 3 liters of saturated CaCl 2 The solution gel was washed with water on the rubber mixer and dried to obtain adhes...

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Abstract

The invention relates to a preparation method of adhesive purpose chloroprene rubber. The preparation method comprises the following steps of: preparation of an oil phase: pouring 100 parts of chloroprene monomer into a sealed container containing 0.15-0.30 part of iodine compound and 3-5 parts of disproportionated rosin and uniformly stirring, wherein the preparation temperature of the oil phaseis 15+ / -2 DEG C; adding the prepared oil phase into a reaction bottle or a reaction kettle, and then adding a prepared water phase under uniformly stirring to emulsify for 20-50 minutes at a temperature of 15-20 DEG C; then adding a redox initiator to carry out a polymerization reaction at a temperature of 5-10 DEG C; when the convert ratio of the chloroprene reaches more than 90 percent, adding phenothiazine used as a terminator once under the stirring and stirring for 15-30 minutes to terminate the polymerization reaction; regulating the pH value to 5-6 by using acetic acid and gelling by using a saturated CaCl2 solution; and washing an obtained product on a rubber mixing mill by water and drying to prepare the adhesive purpose chloroprene rubber. In the preparation method, the iodine compound is used as a molecular weight regulator to synthesize the adhesive purpose chloroprene rubber, and the polymerization has obvious controlled features. An obtained polymer has stable property and narrower molecular weight distribution and can initiate once again for the polymerization of second monomers.

Description

technical field [0001] The invention relates to a preparation method of adhesive neoprene rubber with the characteristics of active radical polymerization. Background technique [0002] Since Matyjaszewski et al first formally proposed the concept of degenerate transfer living radical polymerization in 1995, the research in the field of degenerate transfer living radical polymerization involving iodine-containing compounds has attracted more and more attention. Although researchers and published papers in this field are related to living radical polymerization of initiator-transfer-termination agents, reversible passivation of nitroxide-stabilized radicals, and transition metal-catalyzed atom transfer radical polymerization reactions, based on reversible addition-fragmentation chain Compared with other controllable polymerizations such as living free radical polymerization of transfer agent and controlled free radical polymerization involving diphenylethylene, the number is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/38C08F2/26C08F136/18
Inventor 付志峰谷巨明石艳
Owner BEIJING UNIV OF CHEM TECH
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