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Ultra-high molecular poly(methyl)acrylic acid ester powder for 3D printing and preparation method thereof

An ultra-high molecular weight, acrylate technology, applied in the field of preparation of ultra-high molecular weight polyacrylate powder, can solve the problems of limited application, poor stability, large material size, etc., and achieve the effect of inhibiting thermal decomposition

Active Publication Date: 2014-08-13
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent document 200810007467.3, using the method of staged emulsion polymerization to prepare the polyacrylate copolymer of ultra-high molecular weight, but the poly(meth)acrylate powder material size that this kind of method prepares raw material is big, and stability performance is poor, and this is serious Limiting the application of poly(meth)acrylate powder in 3D printing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] 1) Prepare seed emulsion:

[0067] The polymerization reaction is carried out in a 5-mouth glass-jacketed glass kettle with stirrer, thermometer, condenser, nitrogen conduit and feeding port. The reaction temperature is controlled by a constant temperature water bath. Add 100g of deionized water (total amount 500g) in the reaction kettle, add 150g (total amount 400g) of ethylenic unsaturated monomer-methyl methacrylate, all butyl acrylate 60g and all ethyl acrylate 40g, add emulsifier ten Sodium hexaalkylbenzene sulfonate 10g, oxidizing agent cumene hydroperoxide 0.8g (total amount 1g), all reducing agent ferrous sulfate 0.1g, carving white powder 0.1g, pH value buffering agent sodium hydroxide 1g, metal ion complex Mixture copper sulfate 0.7g, stirred under nitrogen protection and heated up to 25°C.

[0068] 2) Segmented polymerization reaction: observe the heat released by the reaction, and when the temperature rises to 40°C, divide the remaining 250g methyl methacr...

Embodiment 2

[0072] 1) Preparation of seed emulsion: Polymerization is carried out in a 5-mouth glass-jacketed glass kettle with stirrer, thermometer, condenser, nitrogen conduit and feeding port. The reaction temperature is controlled by a constant temperature water bath. Add 150g of deionized water (total amount 500g) in the reaction kettle, add 150g (total amount 400g) of ethylenic unsaturated monomer-methyl methacrylate, all butyl acrylate 50g and all styrene 50g, add emulsifier twelve Sodium alkylbenzene sulfonate 35g, oxidizing agent dicumyl hydroperoxide 1.3g (total amount 1.75g), all reducing agent ferrous sulfate 0.18g, sodium edetate 0.1g, pH buffering agent sodium hydroxide 1 g, 0.8 g of copper sulfate as a metal ion complexing agent, stirred and heated to 25° C. under the protection of nitrogen.

[0073] 2) Segmented polymerization reaction: observe the heat released by the reaction, and when the temperature rises to 40°C, divide the remaining 350g of methyl methacrylate, 65g ...

Embodiment 3

[0077] 1) Prepare seed emulsion:

[0078] The polymerization reaction is carried out in a 5-mouth glass-jacketed glass kettle with stirrer, thermometer, condenser, nitrogen conduit and feeding port. The reaction temperature is controlled by a constant temperature water bath. Add 200g of deionized water (500g in total) in the reaction kettle, add 150g of olefinic unsaturated monomer-methyl methacrylate (400g in total), 70g of all butyl acrylate and 30g of all ethyl acrylate, add emulsifier ten 20g of sodium hexaalkylbenzenesulfonate, 0.12g of tert-butylcumene hydroperoxide as an oxidizing agent (0.14g in total), 0.1g of sodium dithionite as a reducing agent, 0.1g of dithionite powder, and sodium hydroxide as a pH buffering agent 1 g, 0.8 g of copper sulfate as a metal ion complexing agent, stirred and heated to 25° C. under the protection of nitrogen.

[0079] 2) Segmented polymerization reaction: observe the heat released by the reaction, and when the temperature rises to 40...

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Abstract

The invention relates to an ultra-high molecular poly(methyl)acrylic acid ester powder which comprises (methyl)acrylic acid ester, other alkene unsaturated monomer, an emulsifier, an oil-soluble oxidizing agent, a water-soluble reducing agent, an ion complexing agent and a pH buffering agent, wherein based on the total weight of (methyl)acrylic acid ester and other alkene unsaturated monomer, the emulsifier is 10-30%, the oil-soluble oxidizing agent is 0.1-0.4%, the water-soluble reducing agent is 0.01-0.1%, the ion complexing agent is 0.1-2%, and the pH buffering agent is 0.1-1%. The invention also provides a preparation method of the powder and an application of the powder in 3D laser printing. According to the invention, thermal decomposition temperature of the powder rises to 300-315 DEGC. Meanwhile, due to introduction of the oil-soluble oxidizing agent and the water-soluble reducing agent, an aqueous phase reaction is inhibited; and with the combination of the emulsifier, a product with controllable size and relatively uniform particle size can be obtained.

Description

technical field [0001] The invention relates to the field of polymer compounds, in particular to the preparation of an ultra-high molecular weight poly(meth)acrylate powder with high thermal stability, controllable size and uniform particle size, which can be used for 3D printing. Background technique [0002] Selective laser sintering (Selective laser sintering, SLS) is a rapid prototyping technology that uses laser as a heat source to sinter powder materials. Making functional parts with polymer materials is an important development direction of SLS technology and has broad application prospects. Poly(meth)acrylate has good optical properties, as well as good chemical resistance, solvent resistance, and weather resistance. It is widely used in the fields of automobiles, advertising, medicine, communications, and construction. It has great potential in future 3D printing. Very good application prospects. [0003] The molding material used in SLS technology is required to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/14C08F220/18C08F212/08C08F220/06C08F2/26C08F2/30C08F4/40C08L33/12
Inventor 马永梅张晓丹张京楠曹新宇林学春孙文华赵宁董金勇李春成符文鑫
Owner INST OF CHEM CHINESE ACAD OF SCI
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