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Polyurethane curing agent with low free MDI monomer and method for preparing same

A polyurethane curing agent, low free technology, used in polyurea/polyurethane adhesives, adhesives, adhesive types, etc., can solve problems such as health and safety hazards, increase humidity sensitivity, reduce product performance, etc., to achieve savings Low cost, equipment investment and operating cost, low toxicity effect

Inactive Publication Date: 2008-11-19
武汉仕全兴新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In addition, free MDI monomers can cause health and safety hazards and reduce product performance. For example, too much free MDI monomers will undergo dimerization reactions, resulting in the precipitation of insoluble matter, making the product turbid and increasing the sensitivity of the product to humidity. property, the migration of small molecular monomers to the interface leads to a decrease in adhesion, etc.
Therefore, in the curing agent preparation process, the residual amount of MDI monomer should be reduced as much as possible. At present, foreign companies have complicated processes for removing free MDI monomer. The MDI monomer prepolymer with MDI monomer content requires the use of large-scale equipment such as scraper-type thin-film evaporators in the process. These equipment have high initial investment and complex process operations, which greatly increase the product cost.

Method used

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  • Polyurethane curing agent with low free MDI monomer and method for preparing same
  • Polyurethane curing agent with low free MDI monomer and method for preparing same
  • Polyurethane curing agent with low free MDI monomer and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 188g of MDI-50 into a four-necked flask with a condenser and nitrogen protection, add 1.9g of molecular weight regulator diphenyldichlorosilane and 68.5g of ethyl acetate, start stirring, heat up to 50°C, and drop 49g Melting polyol composition (trimethylolpropane 4g, polyester diol 4g, polyester trihydric alcohol 80% solid content 41g), NCO: OH equivalent ratio is 4: 1, adds dropwise in about one hour, Keep warm at 70°C for about 2 hours, add 0.09g of triethylenediamine trimerization catalyst, keep warm at 90°C for reaction, when the total NCO content drops to 12%, cool down to 40°C, add 0.02g of benzoyl chloride inhibitor to terminate reaction.

Embodiment 2

[0036] Add 188g of MDI-100 into a four-necked flask with a condenser and nitrogen protection, add 2.8g of molecular weight modifier di-n-octyldichlorosilane and 69.5g of ethyl acetate, start stirring, heat up to 50°C, drop 51g of molten polyol composition (trimethylolpropane 5g, polyester diol 5g, polyester triol 80% solid content 41g), NCO: OH equivalent ratio is 3.5: 1, dropwise in about one hour , keep warm at 70°C for about 2 hours, add 0.24g of 2,4,6-tris(dimethylaminomethyl)phenol trimerization catalyst, keep warm at 70°C for reaction, when the total NCO content drops to about 12%, add 0.02 g benzoyl chloride inhibitor to terminate the reaction.

Embodiment 3

[0038] Add 188g of MDI-50 into a four-necked flask with a condenser and nitrogen protection, add 2g of molecular weight regulator ethylphenyl dichlorosilane and 68g of butyl acetate, start stirring, heat up to 50°C, and drop 50g Molten polyol composition (trimethylolpropane 5g, polyester triol 80% solid content 45g), NCO: OH equivalent ratio is 5: 1, add dropwise in about one hour, keep warm at 70°C for about 2 hours, Add 0.34g of N, N dimethylbenzylamine trimerization catalyst, keep warm at 80°C, and when the total NCO content drops to about 12%, drop the temperature and add 0.02g of benzoyl chloride polymerization inhibitor to terminate the reaction.

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PUM

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Abstract

The invention discloses a polyurethane firming agent with low free MDI monomers and a method for preparing the same. The invention solves the problems that the prior art has complex MDI polyurethane firming agent preparation process and high equipment investment. The technical proposal comprises the following steps that: the step one, a molecular weight modifying agent is added into a composition of MDI and polylol; prepolymerization reaction is carried out in a solvent, wherein, the equivalent proportion of NCO to OH is 3-5 to 1; and the adding amount of the molecular weight modifying agent is 1 to 1.5 percent of the MDI mass; step two, after the prepolymerization reaction is finished, a trimeric catalyzer is added into the solvent for trimerization reaction; the adding amount of the trimeric catalyzer is 0.1 to 0.3 percent of the residual MDI mass theoretically after the reaction in the step one; after the trimerization reaction is finished, a polymerization inhibitor is added into the solvent to terminate the reaction. The process method has low production cost and simple process equipment; the prepared firming agent has stable storage, low toxicity and performances which can meet various requirements of the firming agent of sizing agent for packing a composite membrane; when the solid content is 75 percent, the content of free MDI monomers is less than 2 percent of the firming agent mass.

Description

technical field [0001] The invention relates to a polyurethane curing agent used in adhesives for solvent-based packaging composite films, in particular to a polyurethane curing agent with low free MDI monomer. Background technique [0002] The food flexible packaging made of composite film material is suitable for people's daily needs due to its light weight, convenience, long shelf life, sanitation, easy storage, easy disassembly and good shelf effect, and is increasingly popular. The properties of these composites depend not only on the selected films but also on the properties of the adhesives used to bond the different film composites together. Usually this type of adhesive includes a main agent and a curing agent. Currently, the commonly used curing agent is a prepolymer of polyols such as toluene diisocyanate (TDI) and trimethylolpropane. Toluene diisocyanate monomer is a colorless transparent liquid with a strong irritating odor and a strong irritating effect on the...

Claims

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Application Information

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IPC IPC(8): C08G18/10C08G18/09C08G18/76C08G18/38C09J175/04
Inventor 王培鹏肖玉新周冬春
Owner 武汉仕全兴新材料科技股份有限公司
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