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A kind of thiopolythiol, preparation method and application in transparent polyurethane material

A polyurethane material and polythiol technology, applied in the preparation of sulfides, organic chemistry, etc., can solve the problems of large dispersion, small refractive index, and unsatisfactory performance.

Active Publication Date: 2020-10-23
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

PC has a high refractive index, but its dispersion is large; while the other two types of dispersion are small, but their refractive index is also small. The highest refractive index of this type of optical glass is only 1.590, and its performance in other aspects is not as good. Therefore, the synthesis of a high-performance optical plastic has become an inevitable trend in the development of optical materials

Method used

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  • A kind of thiopolythiol, preparation method and application in transparent polyurethane material
  • A kind of thiopolythiol, preparation method and application in transparent polyurethane material
  • A kind of thiopolythiol, preparation method and application in transparent polyurethane material

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preparation example Construction

[0050] The preparation method of transparent polyurethane material, comprises the steps:

[0051] After mixing thiopolythiol with isocyanate, polyether polyol, chain extender and additives, after mixing evenly, preheat in microwave for 2 minutes, stir mechanically for reaction, and then pour it into the mold after vacuum defoaming. Curing at room temperature gives colorless and transparent polyurethane. The mass percentage of each raw material of the transparent polyurethane material is: thiopolymercaptan 3-6%, isocyanate 40-50%, polyether polyol 30-40%, chain extender 1-10%, auxiliary agent 1-3% . The isocyanate is isophorone diisocyanate (IPDI), hexamethylene diisocyanate (HDI), hydrogenated diphenylmethane diisocyanate (H 12 MDI) one or any combination. The polyether polyol is one or any combination of PPG2000, PPG3000, PEG2000, and PEG300, and the end group of polyethylene glycol can also be modified with active groups to improve the hardness, impact resistance and othe...

Embodiment 1

[0052] Embodiment 1 Preparation of thiopolythiol

[0053] Preparation of Thiopolyols:

[0054] (1) Accurately weigh 10g of NaOH, 2g of triethylbenzyl ammonium chloride (TEBA), dissolve in 40ml of water and transfer to a 250ml three-necked flask; (2) Place the three-necked flask in an ice-water bath until the temperature drops to Below 5°C, add 9.75 g of 2-mercaptoethanol, stir mechanically, control the temperature of the mixed solution in the reactor below 10°C, and add 23 g of epichlorohydrin dropwise. (3) TLC monitors that the raw materials are completely reacted, neutralize the mixed solution with concentrated hydrochloric acid to pH = 5-6, distill under reduced pressure, remove small molecules, remove salt by suction filtration, and obtain 17.2 g of a colorless and odorless transparent liquid. Yield 64.9%.

[0055] The mass spectrum of thiopolyols is shown as figure 1 As shown, the infrared spectrum is shown in figure 2 shown.

[0056] 1 H NMR characterization resu...

Embodiment 2

[0061] Embodiment 2 Preparation of thiopolythiol

[0062] Preparation of Thiopolyols:

[0063] (1) Accurately weigh 12g NaOH, 2.4g triethylbenzyl ammonium chloride (TEBA), dissolve in 50ml water and transfer to a 250ml three-necked flask; When the temperature is lower than 5°C, add 9.00 g of 2-mercaptoethanol, stir mechanically, control the temperature of the mixed solution in the reactor to be lower than 10°C, and add 25 g of epichlorohydrin dropwise. (3) TLC monitors that the raw materials are completely reacted, neutralize the mixed solution with concentrated hydrochloric acid to pH = 5-6, distill under reduced pressure to remove small molecules, and remove salt by suction filtration to obtain 16.8 g of a colorless and odorless transparent liquid. Yield 60.2%.

[0064] The structural characterization results of thiopolyols are the same as in Example 1.

[0065] Preparation of Thiopolythiols:

[0066] (1) Take 10.8g of the product in 1 into a three-necked flask, add 12.4...

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Abstract

The invention discloses a preparation method of sulfo-polymercaptan and application thereof to transparent polyurethane preparation. The method comprises the following steps: obtaining sulfo-polymercaptan with high sulfur content and high refractive index by a simple and less-pollution method; mixing with a chain extender, a catalyst, an antioxidant and other aids through a proper method, adding IPDI, stirring, and defoaming, thereby obtaining the transparent polyurethane. The method disclosed by the invention is simple, the raw materials are readily available, no organic reagent is used in the S monomer preparation process, damage to the environment and human body is greatly alleviated, and the prepared polyurethane is high in light transmittance, high in refractive index, high in hardness and stable in chemical property.

Description

technical field [0001] The invention relates to a thiopolythiol, a preparation method and an application in transparent polyurethane materials. Background technique [0002] With the advancement of technology and the expansion of application fields, polyurethane has become an all-round polymer and is widely used around the world. The new type of transparent polyurethane, as a kind of polyurethane, overcomes the shortcomings of traditional polyurethane such as opacity and poor heat resistance, and can be used as transparent coatings, heat insulation materials, optical materials, etc., which is a new research direction in recent years. [0003] In recent years, the rapid development of polyurethane in basic research and application development has made it more and more widely used in the field of optics, and as the most important part of optical materials - the development and research of optical plastics is particularly prominent, and has replaced in many fields The use of i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C321/14C07C319/14C08G18/38
CPCC07C321/14C08G18/3868
Inventor 唐果东李乐张宇李荣清支三军
Owner HUAIYIN TEACHERS COLLEGE
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