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Low-viscosity high-reactivity low-volume-contraction modified dipentaerythritol acrylate and preparation method thereof

A high-reactivity, dipentaerythritol technology, applied in the preparation of organic compounds, the preparation of carbamate derivatives, chemical instruments and methods, etc., can solve the adverse effects on the environment and human health, product volatile migration, high volume shrinkage, etc. problems, to achieve the effect of improving light curing efficiency, increasing light curing rate, and low volume shrinkage

Active Publication Date: 2013-11-27
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 dipentaerythritol 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 product flexibility, flexibility, and the adsorption or viscosity of the product application substrate.

Method used

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  • Low-viscosity high-reactivity low-volume-contraction modified dipentaerythritol acrylate and preparation method thereof
  • Low-viscosity high-reactivity low-volume-contraction modified dipentaerythritol acrylate and preparation method thereof
  • Low-viscosity high-reactivity low-volume-contraction modified dipentaerythritol acrylate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0058] Add (127 g, 0.5 mol) dipentaerythritol, (180 g, 2 mol) dimethyl carbonate and (0.56 g, 5 mmol) 1,4-diazabicyclo[2.2.2]octane DABCO into a In a 2000ml reaction flask with a reflux condenser, place the flask in a sand bath in an electric heating mantle, use a temperature controller connected to a thermocouple immersed in the sand bath to control the temperature of the sand bath, use the sand bath to heat the contents of the solution in the flask with stirring To 80 ℃, by stirring, the solid component of the solution in the flask dissolves into a colorless transparent solution, the reaction temperature is maintained at 80 ℃ and continues to stir for 14 hours; the reaction product methanol is continuously distilled out during the reaction, and the excess dicarbonate The methyl ester was distilled out of the reaction bottle, and the remainin...

Embodiment 2

[0060] The cyclic 1,3 propanediol carbonate type modified dipentaerythritol and the diethanolamine reaction synthesis band tertiary amine modified dipentaerythritol polyols by the gained of embodiment 1:

[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, cool to room temperature after the reaction is over, do multiple experiments at the same time under the same conditions as above, 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 the raw material for the next step; the purified product is subjected to FTIR infrared a...

Embodiment 3

[0063] The cyclic 1,3 propanediol carbonate type modified dipentaerythritol and the diisopropanolamine reaction synthesis band tertiary amine modified dipentaerythritol polyol 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 70°C, and the reaction temperature was maintained Stirring was continued at 70 ° C for 3 h, and cooled to room temperature after the reaction was completed.

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Abstract

The invention discloses low-viscosity high-reactivity low-volume-contraction modified dipentaerythritol acrylate and a preparation method thereof. The low-viscosity high-reactivity low-volume-contraction modified dipentaerythritol acrylate has a structural formula as shown in the specification. The degree of functionality of the low-viscosity high-reactivity low-volume-contraction modified dipentaerythritol acrylate is 6-9, the viscosity is 300-2000mPa.s, and the molecular weight is 750-2500, so that the low-viscosity high-reactivity low-volume-contraction modified dipentaerythritol acrylate has very high reactivity, lower viscosity, high molecular weight, low migration, high curing efficiency, low volume contraction rate, good adhesive force and adjustable flexibility, and a prepared coating is good in impact resistance and strong in adhesive force; and the preparation method disclosed by the invention is simple and easy to control, and an obtained product is high in purity and good in performance.

Description

technical field [0001] The invention relates to a modified dipentaerythritol 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C271/16C07C271/18C07C269/06C09D175/14
Inventor 李光照刘和清
Owner JIANGSU RUIYANG CHEM
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