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A kind of preparation method of resin containing water-soluble plasticizer and polyurethane

A plasticizer, water-soluble technology, applied in the field of leather resin, can solve problems such as environmental pollution and damage to workers' health, and achieve the effect of large molecular weight and non-volatile

Active Publication Date: 2018-08-24
姜琪
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because TPU has the characteristics of high tension, high tensile strength, toughness and aging resistance, it is a mature environmental protection material and is widely used in the leather industry. It usually needs to add a large amount of dimethylformamide (DMF) solvent, toluene, Organic solvents such as xylene, acetone, butanone, etc. not only pollute the environment, but also cause damage to the health of workers in related industries, and are flammable and explosive, which can easily cause fire accidents. Therefore, it is urgent to study a more environmentally friendly polyurethane resin.

Method used

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  • A kind of preparation method of resin containing water-soluble plasticizer and polyurethane
  • A kind of preparation method of resin containing water-soluble plasticizer and polyurethane
  • A kind of preparation method of resin containing water-soluble plasticizer and polyurethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Step 1: Add 1 mol of dimethyl glutarate that has been refined and dehydrated into a closed reaction kettle, and simultaneously add 30% sodium methoxide in anhydrous methanol solution containing 0.05 mol of sodium methoxide, and stir under nitrogen protection. 150rpm, then filled with 1.6mol dimethylamine gas, the reaction temperature is 30°C, the reaction time is 7h, the reaction of transesterification into amide occurs, and N 1 ,N 1 ,N 5 ,N 5 - Tetramethylglutaramide and methyl 5-(dimethylamino)-5-oxopentanoate.

[0038] Step 2: Add 85% phosphoric acid aqueous solution containing 0.15 mol of phosphoric acid to the reaction kettle, stir at 150 rpm, and neutralize for 2 hours to generate dimethylamine phosphate and sodium phosphate to remove sodium ions in step 1 and excess dimethylamine.

[0039] Step 3: Move the mixture treated in Step 2 to a filter kettle, and filter to remove dimethylamine phosphate and sodium phosphate.

[0040] Step 4: methanol and water are r...

Embodiment 2

[0044] Step 1: Add 1 mol of dimethyl glutarate that has been refined and dehydrated into a closed reaction kettle, and simultaneously add 30% sodium methoxide in anhydrous methanol solution containing 0.06 mol of sodium methoxide, and stir under nitrogen protection. 200rpm, then filled with 1.8mol dimethylamine gas, the reaction temperature is 40°C, the reaction time is 6h, the reaction of transesterification into amide occurs, and N 1 ,N 1 ,N 5 ,N 5 - Tetramethylglutaramide and methyl 5-(dimethylamino)-5-oxopentanoate.

[0045] Step 2: Add 85% phosphoric acid aqueous solution containing 0.26 mol of phosphoric acid in the above reaction kettle, stir at 200 rpm, and neutralize for 2 hours to generate dimethylamine phosphate and sodium phosphate to remove sodium ions in step 1 and excess dimethylamine.

[0046] Step 3: Move the mixture treated in Step 2 to a filter kettle, and filter to remove dimethylamine phosphate and sodium phosphate.

[0047] Step 4: methanol and water a...

Embodiment 3

[0051] Step 1: Add 1.0 mol of refined 2-methyl-glutaric acid dimethyl ester into a closed reaction kettle, and simultaneously add 30% sodium methoxide in anhydrous methanol solution containing 0.07 mol of sodium methoxide, under nitrogen protection Stir at a stirring speed of 200rpm, then fill with 2.1 mol of dimethylamine gas, the reaction temperature is 50°C, and the reaction time is 6h. The transesterification reaction to amide occurs to generate 2-methyl-5-dimethylcarbamoylvaleric acid methyl ester, methyl 4-methyl-5-dimethylcarbamoylvalerate and dimethyl 2-methyl-1,5-bis(dimethylamino)glutarate.

[0052] Step 2: Add 85% phosphoric acid aqueous solution containing 0.37 mol of phosphoric acid in the above reaction kettle, the stirring speed is 200rpm, and the neutralization reaction time is 2h to generate dimethylamine phosphate and sodium phosphate to remove the sodium ions in step 1 and excess dimethylamine.

[0053] Step 3: Move the mixture treated in Step 2 to a filter...

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Abstract

The invention relates to a preparation method of a resin containing a water-soluble plasticizer and polyurethane. The method comprises the following steps: adding dimethyl glutarate or dimethyl glutarate homologs of which the 2,3,4 carbon sites are provided with methyl or hydroxyl into a closed reaction kettle, charging dimethylamine gas, and carrying out amide ester exchange reaction according to the ratio of the dimethylamine and the dimethyl glutarate or dimethyl glutarate homologs of which the 2,3,4 carbon sites are provided with methyl or hydroxyl of 2.1-2.4; adding a phosphoric acid water solution into the reaction kettle to generate dimethylamine phosphate and sodium phosphate; transferring the mixture treated in the step 2 into a filter kettle, and filtering to remove the dimethylamine phosphate and sodium phosphate; carrying out reduced pressure distillation to remove methanol and water; adding cyclohexyl isocyanate to remove the dimethylamine and water, thereby obtaining the water-soluble plasticizer; adding the water-soluble plasticizer prepared by the steps 1-5 into molten-state polyurethane.

Description

technical field [0001] The invention relates to a leather resin, in particular to a method for preparing a resin containing a water-soluble plasticizer and polyurethane. Background technique [0002] Thermoplastic polyurethane (TPU) is a polymer material formed by the reaction and polymerization of diphenylmethane diisocyanate (MDI), toluene diisocyanate (TDI), macromolecular polyols, and chain extenders. Because TPU has the characteristics of high tension, high tensile strength, toughness and aging resistance, it is a mature environmental protection material and is widely used in the leather industry. It usually needs to add a large amount of dimethylformamide (DMF) solvent, toluene, Organic solvents such as xylene, acetone, butanone, etc. not only pollute the environment, but also cause damage to the health of workers in related industries, and are flammable and explosive, which can easily cause fire accidents. Therefore, it is urgent to study a more environmentally friend...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L75/04C08K5/20C07C231/02
CPCC07C231/02C08K5/20C08K2201/014C08L75/04C07C233/05
Inventor 姜琪
Owner 姜琪
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