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Method for producing an (meth)acrylate syrup

A technology of acrylate and acrylate ester is applied in the field of preparing acrylate slurry, which can solve the problems of poor storage stability of polymer slurry, difficulty in stable preparation of a large amount of slurry, expensive reactor, etc.

Inactive Publication Date: 2007-05-16
LG CHEM LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, polymerization in such a reactor has a problem in that it has a high economic burden since not only the reactor itself is expensive but also the use cost is significant
However, this polymerization method cannot be a fundamental solution because it has the following disadvantages: it causes a large increase in viscosity in the second half of the reaction, exhibits differences in physical properties according to the time point at which the reaction is completed, and since the polymerization inhibitor remains in the In the feed, resulting in poor storage stability of the polymer slurry
However, these methods have a problem in that the polymerization needs to be performed at a relatively high temperature because the reaction proceeds in the absence of an initiator through the transfer of thermally generated radicals so that the reaction rate is very low
However, this high reaction initial temperature has a problem in that it leads to an increase in the highest exothermic reaction of the reaction system, so as to increase the possibility of reaction runaway and make stable preparation of a large amount of slurry difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 570 g of 2-ethylhexyl acrylate (2-EHA), 30 g of acrylic acid (AA), and 0.24 g of the chain transfer agent dodecanemercaptan (n-DDM) into a in a 1-liter four-neck glass reactor. The mixture was heated to a reaction temperature of 70°C while removing dissolved oxygen with a stream of nitrogen for 30 minutes. Then, 0.025 g of 4-(dimethylamino) phenethyl alcohol (DMAPA) as a tertiary amine co-catalyst was added to the mixture and mixed well, 0.036 g of dibenzoyl peroxide initiator dibenzoyl peroxide (BPO) was added thereto, to trigger a reaction.

[0043] The temperature in the reaction was raised to a maximum exothermic temperature of 125° C. in only 8 minutes, and after 30 minutes, was lowered to the reaction temperature set before the reaction started. Thereafter, no increase in the viscosity of the reaction solution occurred, and no exotherm and runaway reaction occurred.

[0044] One hour later, 285 g of 2-ethylhexyl acrylate having room temperature and 15 g of ...

Embodiment 2

[0047] 570 g of butyl acrylate (BA), 30 g of acrylic acid (AA) and 0.24 g of dodecanethiol (n-DDM) were added to the reactor described in the examples. Except that the reaction temperature is 60° C., using 0.06 g of dilauroyl peroxide (LPO) initiator, and adding 285 g of room temperature butyl acrylate and 15 g of acrylic acid for cooling, proceed in the same manner as in Example 1 reaction.

[0048] The temperature in the reaction was raised to a maximum exothermic temperature of 120° C. in only 6 minutes, and after 30 minutes, was lowered to the reaction temperature set before the reaction started. Thereafter, no increase in the viscosity of the reaction solution occurred, and no exotherm and runaway reaction occurred. The concentration of solids in the partially polymerized slurry thus prepared was 50.4%, and the slurry had a viscosity of 11,000 centipoise (cP) and a molecular weight of 350,000.

Embodiment 3

[0050] The same monomers as in Example 1 were charged into the reactor described in Example 1 in the same amount as in Example 1. In addition to using 0.58g of pentaerythritol four (3-mercapto) propionate as chain transfer agent, 0.036g of dibenzoyl peroxide initiator and 0.020g of N,N'-dimethyl-p-toluidine as Except for the co-catalyst, the reaction was carried out in the same manner as in Examples.

[0051] The temperature in the reaction was raised to a maximum exothermic temperature of 122°C in only 8 minutes, and after 30 minutes, was lowered to the reaction temperature set before the reaction started. Thereafter, no increase in the viscosity of the reaction solution occurred, and no exotherm and runaway reaction occurred. The concentration of solids in the partially polymerized slurry thus prepared was 47.8%, and the slurry had a viscosity of 7,700 centipoise (cP) and a molecular weight of 330,000.

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PUM

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Abstract

The invention discloses a method for producing (meth)acrylate syrup, the method comprising initiating polymerization using the following components at a temperature of 50-80 DEG C: a (meth)acrylate ester monomer, a chain transfer agent, a diacyl peroxide initiator, and 0.5-3.0 moles, based on 1 mole of the diacyl peroxide initiator, of a tertiary amine cocatalyst. In the disclosed method, a reaction runway does not occur even in bulk polymerization, it is easy to control molecular weight and it is possible to form a high-molecular weight (meth)acrylate syrup without stirring failure.

Description

technical field [0001] The invention relates to a method for preparing (meth)acrylate syrup. More specifically, the present invention relates to a method for preparing (meth)acrylate syrup in which reaction runaway does not occur even in bulk polymerization, molecular weight control is easy, and formation of high molecular weight (meth)acrylate is possible slurry. Background technique [0002] In the prior art, since the (meth)acrylic resin composition has excellent transparency and is easy to control its cured material to adhere to various substrates, it has been used in applications such as adhesive sheets, protective coatings and adhesive various applications of the agent. Although these materials for their respective applications become highly functional, much energy is required to remove residues for their preparation using solution polymerization, emulsion polymerization or suspension polymerization. In addition, in the use of this polymerization method, it is diffi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/02C08F290/04
CPCC08F4/58C08F2/38C08F290/04C08F220/14C08F2/02C08F265/06C08F20/06C08G63/00
Inventor 李在官金鲁马张锡基
Owner LG CHEM LTD