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A kind of preparation method of organosilicon cationic waterborne polyurethane

A technology of water-based polyurethane and silicone, applied in the chemical industry, can solve the problems of water resistance, solvent resistance, heat resistance and gloss, poor mechanical properties of water-based polyurethane, easy yellowing of water-based polyurethane, etc., and meet the requirements of reaction equipment. High, improved water resistance and stretch resistance, easy to separate effect

Active Publication Date: 2016-07-06
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aromatic isocyanates such as TDI and MDI synthesized water-based polyurethane are prone to yellowing, and aliphatic isocyanates such as HMDI can solve this problem well, but the use of chain extenders containing primary, secondary and tertiary amines also causes yellowing of water-based polyurethane important reason for
Due to the introduction of hydrophilic groups into the macromolecular structure during the synthesis of water-based polyurethane, and most of the water-based polyurethanes are linear polymers, although there are physical cross-links formed by hydrogen bonds inside, they lack chemical cross-links, so the mechanical properties of water-based polyurethane are relatively low. Poor, water resistance, solvent resistance, heat resistance and gloss are not ideal

Method used

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  • A kind of preparation method of organosilicon cationic waterborne polyurethane
  • A kind of preparation method of organosilicon cationic waterborne polyurethane
  • A kind of preparation method of organosilicon cationic waterborne polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] A preparation method of organosilicon cationic waterborne polyurethane, the steps are as follows:

[0059] (1) Take 30ml of saturated sodium hydroxide solution and add it to a 500ml four-neck flask with reflux and a thermometer, heat up to 40°C, mix 15.466g (0.2021mol) of allyl chloride and 14.683g (0.2008mol) of diethylamine Drop by drop into a four-necked bottle, the time for dropping is 90min, heat up to 65°C, keep stirring at normal pressure for 16h, cool to room temperature, filter to obtain the filtrate, let it stand, separate the supernatant with a separatory funnel, Distilled under normal pressure to obtain a fraction with a boiling point of 104-106°C to obtain diethylallylamine; the product yield is 61%, and the purity is 99.2%;

[0060] The distilled fraction with a boiling point below 70°C can be reused;

[0061] (2) Take 5.170g of acidified cation exchange resin, 16.416g (0.1222mol) of tetramethyldisiloxane (HMM) and 35.594g (0.1200mol) of octamethylcyclote...

Embodiment 2

[0067] A preparation method of organosilicon cationic waterborne polyurethane, the steps are as follows:

[0068] (1) Take 30ml of saturated sodium hydroxide solution and add it to a 500ml four-neck flask with reflux and a thermometer, heat up to 40°C, mix 15.466g (0.2021mol) of allyl chloride and 14.683g (0.2008mol) of diethylamine Drop by drop into a four-necked bottle, the time for dropping is 90min, heat up to 65°C, keep stirring at normal pressure for 16h, cool to room temperature, filter to obtain the filtrate, let it stand, separate the supernatant with a separatory funnel, Distilled under normal pressure to obtain a fraction with a boiling point of 104-106°C to obtain diethylallylamine; the product yield is 61%, and the purity is 99.2%;

[0069] The distilled fraction with a boiling point below 70°C can be reused;

[0070] (2) Take 5.908g of acidified cation exchange resin, 13.579g (0.1000mol) of tetramethyldisiloxane (HMM) and 44.493g (0.15mol) of octamethylcyclotetr...

Embodiment 3

[0076] A kind of preparation method of organosilicon cationic waterborne polyurethane, step is the same as embodiment 1, difference is:

[0077] The temperature of the heat preservation reaction in the step (1) is 60 DEG C, and the heat preservation reaction time is 18h;

[0078] In step (2), the reaction temperature is 90°C, and the reaction time is 10h;

[0079] In step (3), the reaction temperature is 30°C, and the reaction time is 4h;

[0080] In step (4), the reaction temperature is 60°C, and the reaction time is 48h;

[0081] In step (5), the reaction temperature between polytetrahydrofuran diol and 4,4'-dicyclohexylmethane diisocyanate is 40°C, and the reaction time is 4h; The temperature is 40°C and the reaction time is 3h.

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Abstract

The invention relates to a preparation method for organosilicone positive ion waterborne polyurethane. The preparation method comprises the following steps: (1) reacting diethylamine with allyl chloride in the presence of an alkaline to generate diethyl allylamine; (2) carrying ring opening on D4 under the effect of a catalyst and blocking by using HMM (hexamethylmelamine) to generate dihydro-blocked polysiloxane; (3) carrying out hydrosilylation reaction on dihydro-blocked polysiloxane and diethyl allylamine; (4) carrying out quaternization reaction on the production of the addition reaction and chloropropanol; and (5) generating a prepolymer through reaction between HMDI and PTMEG1000 and extending chains in water by using the quaternization product to generate the organosilicone positive ion waterborne polyurethane. The preparation method provided by the invention is simple and convenient to operate, mild in reaction condition, free of carbonization and products are easily separated and recycled. Firstly, polysiloxane with amido at two terminals is salified and then chains are extended, and the conventional step of salifying positive ions with an acid and then neutralizing is cancelled, so that use of a nitrogen-containing chain extender is reduced, the cost is saved and the problem that positive ion polyurethane gets yellow is prevented.

Description

technical field [0001] The invention relates to a preparation method of organosilicon cationic waterborne polyurethane, which belongs to the technical field of chemical industry. Background technique [0002] Cationic water-based polyurethane inherits the advantages of water-based polyurethane (WPU) such as non-flammability, non-toxicity, and environmental friendliness. At the same time, because the ions formed by it are quaternary ammonium salts, the particles are positively charged, which is the same as the charge carried by dust in the air, and has a certain It has good dustproof effect; its bonding performance is also good, and it can be used as an adhesive for some substrates; in addition, cationic water-based polyurethane also has a certain bactericidal effect and can be widely used as a fabric finishing agent. However, the process of salting the prepolymer is more complicated, the cost is higher, the product yellows seriously, and the emulsified product is sometimes n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/75C08G18/48C08G18/61C08G77/388C08G77/385C08G77/12
CPCC08G18/10C08G18/3206C08G18/4854C08G18/61C08G77/12C08G77/385C08G77/388C09D175/08C08G18/6517
Inventor 李俊英崔月芝郝传明张文郁陶芙蓉崔晓
Owner QILU UNIV OF TECH
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