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Preparation method of polyfunctional branched polyurethane slurry for photocuring direct-write forming

A technology of polyurethane slurry and direct writing molding, which is applied in the field of light-curing materials, can solve the problems of low viscosity of polyurethane acrylate and cannot meet the requirements of direct writing molding, and achieve fast light curing speed, high production efficiency, good personnel friendliness and The effect of environmental significance

Active Publication Date: 2018-06-29
LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the patent document CN201511019707.8 discloses "ultraviolet light-curable polyurethane acrylate and its preparation method". In this patent document, diisocyanate, diol, hydroxy acrylate and triethylamine are used as raw materials to synthesize a compound with a higher glass transition temperature. A new type of UV-curable urethane acrylate, but the viscosity of urethane acrylate obtained by this method is low, which cannot meet the needs of direct writing molding

Method used

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  • Preparation method of polyfunctional branched polyurethane slurry for photocuring direct-write forming
  • Preparation method of polyfunctional branched polyurethane slurry for photocuring direct-write forming
  • Preparation method of polyfunctional branched polyurethane slurry for photocuring direct-write forming

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Step 1. Under nitrogen protection, add 7.50g diphenylmethane diisocyanate (MDI, 30mmol), 18.96mg dibutyltin dilaurate (DBTDA, 0.03mmol) and 9.18g anhydrous 1,4-dioxane In the reaction bottle, stir with a magnetic heating stirrer at a stirring speed of 100rpm. After heating to 70°C, slowly add 1.68g of trityl alcohol (10mmol) dropwise. Branched intermediate (formula 1);

[0036] Step 2, under the protection of nitrogen, add 7.50g diphenylmethane diisocyanate (MDI, 30mmol), 18.96mg dibutyltin dilaurate (DBTDA, 0.03mmol) and 16.44g anhydrous 1,4-dioxane In the reaction flask, stir with a magnetic heating stirrer at a stirring speed of 100rpm. After heating to 70°C, dissolve 3.24mg of p-benzoquinone (0.03mmol) in 8.94g of pentaerythritol triacrylate (30mmol), and slowly add it dropwise to the reaction flask In, after the dropwise addition was completed, the reaction was continued for 3 hours to obtain an acrylate intermediate (formula 2) with an isocyanate group;

[0037] S...

Embodiment 2

[0043] Step 1. Under nitrogen protection, add 5.22g of toluene diisocyanate (MDI, 30mmol), 18.96mg of dibutyltin dilaurate (DBTDA, 0.03mmol) and 6.90g of anhydrous 1,4-dioxane into the reaction flask , stirring with a magnetic heating stirrer, the stirring speed is 100rpm, after heating to 70°C, slowly add 1.68g of triphenylmethanol (10mmol) dropwise, after the dropwise addition is completed, continue the reaction for 3h, and obtain the isocyanate-terminated branched intermediate body (Formula 1);

[0044] Step 2. Under nitrogen protection, add 5.22g of toluene diisocyanate (MDI, 30mmol), 18.96mg of dibutyltin dilaurate (DBTDA, 0.03mmol) and 9.12g of anhydrous 1,4-dioxane into the reaction flask , magnetic heating stirrer stirring, stirring speed 100rpm, after heating to 70 ° C, 3.30mg of hydroquinone (0.03mmol) was dissolved in 3.90g of hydroxypropyl acrylate (30mmol), slowly added dropwise to the reaction flask, dropwise After the addition was completed, the reaction was co...

Embodiment 3

[0051] Step 1. Under nitrogen protection, add 6.40g p-phenylene diisocyanate (40mmol), 6.32mg dibutyltin dilaurate (DBTDA, 0.01mmol) and 8.88g anhydrous ethylene glycol dimethyl ether into the reaction flask, and magnetically heat Stir with a stirrer at a stirring speed of 150 rpm. After heating to 60° C., slowly add 2.48 g of naphthalene tetramethanol (10 mmol) dropwise. After the dropwise addition is completed, continue the reaction for 2 h to obtain an isocyanate-terminated branched intermediate (Formula 1 );

[0052] Step 2, under the protection of nitrogen, add 6.40g p-phenylene diisocyanate (40mmol), 6.32mg dibutyltin dilaurate (DBTDA, 0.01mmol) and 11.60g anhydrous ethylene glycol dimethyl ether into the reaction flask, magnetic heating Stir with a stirrer at a stirring speed of 150rpm. After heating to 60°C, dissolve 4.96mg of p-methoxyphenol (0.04mmol) in 5.20g of hydroxyethyl methacrylate (40mmol), and continue the reaction for 2 hours after the dropwise addition is ...

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Abstract

The invention discloses a preparation method of a polyfunctional branched polyurethane slurry for photocuring direct-write forming. The preparation method comprises the following steps of enabling isocyanate, aryl polyols, dihydric alcohol and hydroxyl acrylate to react, and adjusting the types and proportional ratio of the four raw materials, so as to obtain a direct-write slurry with adjustableviscosity, wherein the direct-write slurry is suitable for the direct-write forming under different conditions; the direct-write slurry does not contain any solvent, and the solid content reaches 100%; the photocuring rate is quick, the production efficiency is high, and the like; after extruding, the curing time is obviously shortened, and the production efficiency is improved. The preparation method of the polyfunctional branched polyurethane slurry for the photocuring direct-write forming has the advantages that the technology is simple; by adding a proper amount of end blocking agent, theisocyanate group is controlled to completely react and block the end; the adding of active thinner and additive with low molecular weight is not needed; the good person-friendly effect and environment-protection meaning are realized.

Description

technical field [0001] The invention relates to the technical field of photocurable materials, in particular to a method for preparing UV photocurable multifunctional branched polyurethane slurry for direct writing molding. Background technique [0002] Direct writing molding is an important rapid prototyping technology, which was first reported by the Sandia National Laboratory in the United States. It can be extruded from the nozzle to form a linear fluid by controlling the rheological properties of the slurry, and the slurry is automatically controlled by the computer. The device changes its trajectory on the x-y platform, and precisely forms the first layer structure on the substrate according to the pre-design. Then the ink delivery device is moved upwards to the height determined by the design proposal, and the second layer of slurry is formed on the structure formed by the first layer of forming slurry. This step is then repeated until the entire three-dimensional st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/66C08G18/67C08G18/32C08G18/48
CPCC08G18/3215C08G18/4833C08G18/672C08G18/673C08G18/6677
Inventor 张帅李婧陈素芬龚晓婷李波尹强刘梅芳李洁刘一杨
Owner LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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