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Method for preparing polymer crystal at low temperature by using ultraviolet polymerization

A UV and polymer technology, applied in the direction of ester copolymer adhesives, adhesive types, coatings, etc., can solve the problems without further research on the microscopic morphology of the photopolymerization system, and achieve the goal of broadening the temperature range Effect

Inactive Publication Date: 2011-11-23
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] All of the above studies have only studied the kinetics of the photopolymerization system, and have not studied the microscopic morphology of the photopolymerization system at low temperature.

Method used

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  • Method for preparing polymer crystal at low temperature by using ultraviolet polymerization
  • Method for preparing polymer crystal at low temperature by using ultraviolet polymerization
  • Method for preparing polymer crystal at low temperature by using ultraviolet polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 0.03g of photoinitiator 1173 and add it to 6.00g of HDDA to prepare a photopolymerization system with a mass ratio of initiator to monomer of 1:200. Ultrasonic vibration at room temperature for 5 minutes makes the system uniformly dispersed. Inject the system into the mold with a 1mL needle tube, put it into a low-temperature constant temperature tank, and keep the temperature at -25°C, and use 30mW / cm 2 The ultraviolet light irradiates the polymerization system for 1min, and the polymerized sample is soaked in acetone for 48h. After the treatment, the sample is prepared and the crystal structure can be observed under the high-resolution transmission electron microscope. The interplanar distance d=0.2857nm. In cold climates in winter, low-temperature curing light-curing materials can be applied to coatings at low temperatures.

Embodiment 2

[0025] Take 0.003g of photoinitiator 184, add it to 6.00g of HDDA, and prepare six sets of photopolymerization systems with a mass ratio of initiator to monomer of 1:200, numbered (1) to (6), and ultrasonically shake at room temperature for 100 minutes. Mix the system evenly. The system was injected into the mold with a 1 mL needle. Put the polymerization systems numbered (1), (2) and (3) into a low-temperature thermostat, and drop the temperature from room temperature to -25 °C, -10 °C and 0 °C at a rate of 1.6 °C / min, respectively. 80mW / cm 2 The ultraviolet light was irradiated on the polymerization system for 50min. Put the polymerization systems numbered (4), (5) and (6) into the low-temperature constant temperature baths whose temperature has been stabilized at -25°C, -10°C and 0°C respectively, and use a light intensity of 80mW / cm 2 The ultraviolet light was irradiated on the polymerization system for 50min. Put the polymerized samples (1) to (6) into acetone and soa...

Embodiment 3

[0027] Take 0.300g of photoinitiator 819 and add it to 6.00g of HDDA to prepare a photopolymerization system with a mass ratio of initiator to monomer of 1:20. Ultrasonic vibration at room temperature for 15 minutes makes the system uniformly dispersed. Inject the system into the mold with a 1mL needle tube, place it in a low-temperature constant temperature bath, keep the temperature at -30°C, and use a light intensity of 45mW / cm 2 The system was irradiated with ultraviolet light for 15 minutes to obtain polymer crystals. Its interplanar spacing d=0.3458nm can be used as a low-temperature adhesive material.

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Abstract

The invention relates to a method for preparing a polymer crystal, and belongs to the field of ultraviolet polymerization method. The method is characterized in that: the method comprises three polymerization reactions according to the following three directions: (1) mixing a photopolymerizable monomer and small amount of an initiator according to a certain ratio, followed by carrying out polymerization under the ultraviolet irradiation; (2) mixing two photopolymerizable monomers and small amount of an initiator according to a certain ratio, followed by carrying out polymerization under the ultraviolet irradiation through copolymerization reaction; (3) dissolving a photopolymerizable monomer in a certain amount of a solvent, followed by adding small amount of an initiator according to a certain ratio to carry out polymerization under the ultraviolet irradiation; then the prepared photopolymerizable system is placed at a low temperature less than -80-0 DEG C to enable the prepared photopolymerizable system to be converted from the transparent liquid to the crystal, then 30-80 mW / cm<2> of the ultraviolet is adopted to carry out irradiation for 1-50 minutes to obtain the polymer crystal. The method provided by the present invention is easy to be controlled, has simple steps, simple post treatment operation, and no pollution to environment.

Description

technical field [0001] The invention relates to the research on the method of preparing polymer crystals at low temperature by means of ultraviolet light polymerization. Background technique [0002] With the increasing commercial application of light-curing products in different fields, such as coatings, inks, microelectronics and dental restoration materials, light-curing technology has attracted more and more attention. Photocuring technology rapidly converts liquid multifunctional monomers and oligomers into solid polymers by irradiation with ultraviolet light in the presence of an initiator. The performance of the cured product can be affected by many factors, such as the structure and type of photoinitiator, monomer structure and polymerization temperature, etc. [0003] As far as the influence of temperature on the photopolymerization system is concerned, many researchers have studied the influence of temperature on the photopolymerization kinetics of acrylate and me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C08F122/14C08F122/20C08F222/14C08F220/32C08F120/28C09D135/02C09D133/14C09J135/02C09J133/14
Inventor 聂俊崔明马贵平
Owner BEIJING UNIV OF CHEM TECH
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