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Branched aqueous carbodiimide type crosslinking agent and preparation method thereof

A carbodiimide type and cross-linking agent technology, applied in the direction of organic chemistry, can solve the problems of weakened cross-linking activity, cross-linking activity and water solubility/dispersibility at the same time, and achieve simple preparation process and excellent water solubility Sexuality/dispersibility, low color change index effect

Inactive Publication Date: 2018-11-23
四川创世新琰科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing carbodiimide-type water-based cross-linking agent has a regular linear structure and no branching. During the preparation process, the viscosity of the system will increase rapidly with the increase of the degree of polymerization. If the degree of polymerization is increased to enhance the cross-linking activity , the water solubility / dispersibility will decrease again, and if the water solubility / dispersibility is increased, the crosslinking activity will be weakened with the decrease of the degree of polymerization, so the crosslinking activity and water solubility / dispersibility cannot be taken into account at the same time

Method used

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  • Branched aqueous carbodiimide type crosslinking agent and preparation method thereof
  • Branched aqueous carbodiimide type crosslinking agent and preparation method thereof
  • Branched aqueous carbodiimide type crosslinking agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of branched waterborne carbodiimide crosslinking agent

[0025] 61.5g triphenylmethane triisocyanate, 263.7g dicyclohexylmethane diisocyanate, 3.25g 1-phenyl-2-cyclobutene 1-oxide and 3.25g phosphite were mixed with β-(3,5- The mixture of di-tert-butyl-4-hydroxyphenyl) octadecyl propionate is added to the reactor together, in which, the phosphite and β-(3,5-di-tert-butyl-4-hydroxyphenyl) Octadecyl propionate is mixed at a molar ratio of 1:2.3, and then press 25cm 3 The flow rate of / min was passed into hydrogen protection, stirred and reacted at 160°C for 5h, and then the temperature in the reactor was lowered to 100°C, and 3.25g of trifluoroalkanoic acid trimethylsilicate was added, and the stirred reaction was continued for 1h before adding 109.6g of sodium 3-allyloxy-2-hydroxyl-1-propanesulfonate, and continue to stir for another 2h; finally lower the temperature in the reactor to below 35°C, add 600.5g of distilled water to dilute to a solid content of ...

Embodiment 2

[0027] Preparation of branched waterborne carbodiimide crosslinking agent

[0028] 27.3 g of pentaerythritol, 269.8 g of trimethyl-1,6-hexamethylene diisocyanate, 2.97 g of 3-methyl-2-cyclobutene 1-oxide and 2.97 g of phosphite were mixed with 1,3, A mixture of 5-trimethyl-2,4,6-(3,5-di-tert-butyl-4-hydroxybenzyl)benzene is added to the reactor together, in which phosphite and 1,3,5- Trimethyl-2,4,6-(3,5-di-tert-butyl-4-hydroxybenzyl)benzene is mixed at a molar ratio of 1:2.3, and then press 28cm 3 The flow rate of / min was passed into hydrogen protection, and the reaction was stirred at 138°C for 8h, and then the temperature in the reactor was lowered to 90°C, and 2.97g of trimethylsilyl methanesulfonate was added, and the stirring reaction was continued for 0.5h before adding 130g of sodium 3-hydroxy-1-propanesulfonate, and continue to stir for 2.5 hours; finally, the temperature in the reactor is lowered to below 35°C, and 601g of distilled water is added to dilute to a so...

Embodiment 3

[0030] Preparation of branched waterborne carbodiimide crosslinking agent

[0031] 23.5g of tetraethylenepentamine, 310.6g of diphenylmethane diisocyanate, 3.34g of 3-methyl-2-cyclobutene 1-oxide and 3.34g of phosphite were mixed with β-(3,5-ditertiary The mixture of butyl-4-hydroxyphenyl)propionate isooctanol is added to the reactor together, wherein, phosphite and β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate are Octanol esters are mixed at a molar ratio of 1:2.3, and then press 30cm 3 The flow rate of / min was passed into hydrogen protection, and the reaction was stirred at 120°C for 5.5h, and then the temperature in the reactor was lowered to 90°C, and 3.34g of diethyl trimethylsilicon phosphate was added, and the stirring reaction was continued for 0.5h before Add 83.23g of sodium hydroxymethanesulfonate, and continue to stir and react for 2 hours; finally, reduce the temperature in the reactor to below 35°C, add 600.1g of distilled water to dilute to a solid content o...

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Abstract

The invention relates to a branched aqueous carbodiimide type crosslinking agent and a preparation method thereof, and belongs to the technical field of polymer materials. The crosslinking agent has the structural formula as shown in the specification, wherein R1 is a polyfunctional compound group getting rid of an effective functional group reactive with isocyanate; R2 is a diisocyanate group getting rid of two isocyanato; R3 is a hydrophilic compound group getting rid of an effective functional group reactive with isocyanate; CB1 is a chemical bond formed by reacting an effective functionalgroup reactive with isocyanate on R1 with isocyanate; CB2 is a chemical bond formed by reacting an effective functional group reactive with isocyanate on R3 with isocyanate; m is an integer greater than 2; n is equal to 1-10. The cross-linking agent has good water solubility / dispersibility and low color change index, and can be used for crosslinking of aqueous coatings and hydrolysis resistance ofpolyester polymer materials. The preparation process is simple, the equipment requirements are not high, the cost is low, and thus the preparation method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a branched water-based carbodiimide crosslinking agent and a preparation method thereof. Background technique [0002] In recent years, water-based resin has become a new favorite in the field of coating applications because it conforms to the concept of green and safe environmental protection, and has excellent performance in adhesion, film formation, and functional modification. Although water-based resin has many advantages, its low degree of crosslinking, weak adhesion to some substrates, unsatisfactory mechanical strength, poor solvent resistance and hydrolysis resistance, etc., also restrict its application to a certain extent. The use of water-based cross-linking agents can make up for these defects of water-based resins. Among them, carbodiimide-type water-based cross-linking agents have the advantages of safety, environmental protection, non-toxicit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C267/00C08K5/29
CPCC07C267/00C08K5/29
Inventor 张勇张风顺李雪雁
Owner 四川创世新琰科技有限责任公司
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