Low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate and preparation method thereof

A technology of pentaerythritol acrylate and high reactivity, which is applied in the preparation of organic compounds, preparation of carbamic acid derivatives, chemical instruments and methods, etc., and can solve the adverse effects on the environment and human health, product volatile migration, toxicity and irritation and other problems, to achieve the effect of improving photocuring efficiency, increasing photocuring rate, and high molecular weight

Active Publication Date: 2013-12-11
JIANGSU RUIYANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the higher viscosity makes this type of resin used in UV-curable coatings, it is necessary to add low molecular weight reactive diluents with relatively small viscosity to reduce the viscosity of the coating composition to a viscosity of not more than 4Pa.s and preferably not more than 2.5 Viscosity of Pa.s at room temperature. Although low molecular weight reactive diluents have low viscosity and good dilution effect, most of them have low vapor pressure, toxicity and irritation, and will remain in the product after the light is over, causing adverse effects on the environment and human health. impact, and the cost is high, the operation is complicated, and the obtained product is easy to volatilize and migrate, and the loss is large
[0006] The common pentaerythritol acrylate has the disadvantages of high viscosity, poor dilution, hard and brittle cured film, high volume shrinkage affecting adhesion, poor impact resistance (poor flexibility), and poor flexibility. There are great defects in flexibility, flexibility, and the adsorption or stickiness of the product application substrate

Method used

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  • Low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate and preparation method thereof
  • Low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate and preparation method thereof
  • Low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Preparation of cyclic 1,3 propanediol carbonate type modified pentaerythritol from pentaerythritol and dimethyl carbonate:

[0058] Add (68 g, 0.5 mol) pentaerythritol, (180 g, 2 mol) dimethyl carbonate and (0.56 g, 5 mmol) 1,4-diazabicyclo[2.2.2]octane DABCO to a device equipped with electric stirring and water-cooled reflux In the 2000ml reaction flask of the condenser, place the flask in the sand bath in the electric heating mantle, use the temperature controller connected to the thermocouple immersed in the sand bath to control the temperature of the sand bath, so that the solution substance in the flask is 80 ° C, by stirring , the solid components of the solution substance in the flask were dissolved into a colorless transparent solution, and the reaction temperature was maintained at 80°C and continued to stir for 14 hours. During the reaction, the reaction product methanol was continuously distilled out, and the excess dimethyl carbonate was distilled out after t...

Embodiment 2

[0060] The cyclic 1,3 propanediol carbonate type modified pentaerythritol and the diethanolamine are reacted to synthesize the modified pentaerythritol polyol with tertiary amine by embodiment 1 gained:

[0061] Before cooling the reaction product in the flask of Example 1 to room temperature, add (105g, 1mol) diethanolamine and 600ml cyclohexane, under the action of electric stirring, the solution in the flask is slowly heated to 70°C, and the reaction temperature is maintained at 70°C Continue to stir for 3 hours, after the reaction is over, cool to room temperature; under the same conditions as above, do multiple experiments at the same time, one of the obtained products is purified by ethanol and water precipitation, recrystallization, etc., and is separated by silica gel chromatography (n-hexane: acetic acid Ethyl ester = 4:1), the rest of the resulting product is not further processed as a raw material for the next step; the purified product is subjected to FTIR infrared ...

Embodiment 3

[0063] The cyclic 1,3 propanediol carbonate type modified pentaerythritol and diisopropanolamine reaction synthesis band tertiary amine modified pentaerythritol polyols by embodiment 1 gained:

[0064] Before cooling the reaction product in the flask of Example 1 to room temperature, (133g, 1mol) diisopropanolamine and 600ml cyclohexane were added, and under the action of electric stirring, the solution in the flask was slowly heated to 75°C, and the reaction temperature was maintained Stirring was continued at 75°C for 3h, the reaction was completed and cooled to room temperature.

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Abstract

The invention discloses low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate and a preparation method thereof. The low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate has a structural formula as shown in the specification. The functionality of the low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate is 4-6, the viscosity is 40-70mPa.s, and the molecular weight is 750-2500, so that the low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate is very high in reactivity, low in viscosity, high in molecular weight, low in migration, high in curing efficiency, low in volume shrinkage ratio, good in adhesive force and adjustable in flexibility, and a prepared paint is good in impact resistance and strong in adhesive force. The preparation method disclosed by the invention is simple and easy to control, and the obtained product is high in purity and good in performance.

Description

technical field [0001] The invention relates to a modified pentaerythritol acrylate with low viscosity, high reactivity and low volume shrinkage and a preparation method thereof. Background technique [0002] Light curing technology has the advantages of fast curing, energy saving and time saving, low solvent release, low curing temperature, small equipment size, low investment, etc. Its application fields have developed from the initial wood coating to plastic decoration, metal parts coating, medical treatment, etc. Apparatus, electronic components, information recording media, photosensitive printing, plastic materials and optical fibers and other industrial production fields, it mainly appears in the form of UV coatings, UV inks, UV adhesives, etc. [0003] UV curing materials are composed of photosensitive prepolymers (oligomers), reactive diluent monomers, photoinitiators and various additives (pigments, fillers, defoamers, etc.). Prepolymer is the basic resin of the U...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C271/16C07C271/64C07C269/06C09D175/14C09D7/12
Inventor 李光照刘和清
Owner JIANGSU RUIYANG CHEM
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