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Preparation method of sulfonate amphoteric polyurethane emulsion

A polyurethane emulsion and sulfonate type technology, which is applied in the field of polymer material preparation, can solve the problems of long reaction time and difficulty in continuous production, and achieves convenient control of emulsification degree, less amount of sulfonate, good appearance and heavy weight present effect

Inactive Publication Date: 2010-02-03
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, there are few reports on amphoteric polyurethanes, and these reports are all amphoteric polyurethanes based on dihydroxymethylpropionic acid (DMPA) and tertiary amino groups. Due to the characteristics of dihydroxymethylpropionic acid (DMPA), this type of polyurethane is mainly There are the following disadvantages: A. The reaction time is long, generally about 8 hours from raw materials to products; B. Continuous production is difficult, and DMPA is used as a hydrophilic chain extender, and the prepolymer material must be transferred from the reactor to the emulsification The emulsion is prepared by high-speed shear emulsification and dispersion in the barrel, and then returned to the still for desolventization; C, amine neutralizer has a strong smell, and DMPA is used as a hydrophilic chain extender, which cannot be directly emulsified, and amines are required Emulsify after neutralizing -COOH in DMPA
It is precisely because of this that when this amphoteric polyurethane is used for protein model compounds, it is limited when it is used as a carrier for biological macromolecules

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053](1), under the protection of dry nitrogen, the number average molecular weight after vacuum dehydration is 1000, the polyoxypropylene diol (N-210) 30g of hydroxyl value 1.96mmol / g, isophorone isocyanate (IPDI) 19.98 g was added to the reaction vessel, and the reaction was carried out at 85°C-100°C under mechanical stirring for 2 hours;

[0054] (2) Lower the system temperature to 40°C-60°C, add 2.30g of diethylene glycol (DEG), then add 5mL of acetone and catalyst dibutyltin dilaurate (T-12) 0.03-0.05g (3 drops ), stannous octoate (T-9) 0.03-0.05g (3 drops), under mechanical stirring, control the temperature at 55°C to 75°C for 2h;

[0055] (3) Reduce the temperature of the system to below 60°C, add 2.50g of cationic chain extender N-methyldiethanolamine (DB), and add 15mL of acetone to prevent gelation caused by excessive viscosity, and control the temperature at 40-60°C Reaction between ℃ for 1h;

[0056] (4) Add 3.50 g of sodium ethylenediaminoethanesulfonate to the...

Embodiment 2

[0058] (1), under the protection of dry nitrogen, 30g of polyoxypropylene diol (N-210) with a number average molecular weight of 1000 and a hydroxyl value of 1.96mmol / g after vacuum dehydration, and 26.26g of isophorone isocyanate (IPDI) Add it into the reaction container, and control it at 85°C-100°C under mechanical stirring for 2h;

[0059] (2) Lower the system temperature to 40°C-60°C, add 3.97g of diethylene glycol (DEG), then add 7mL of acetone and catalyst dibutyltin dilaurate (T-12) 0.03-0.05g (3 drops ), stannous octoate (T-9) 0.03-0.05g (3 drops), under mechanical stirring, control the temperature at 55°C to 75°C for 2h;

[0060] (3) Reduce the temperature of the system to below 60°C, add 2.81g of cationic chain extender N-methyldiethanolamine (DB), and add 15mL of acetone to prevent gelation caused by excessive viscosity, and control the temperature at 40-60°C Reaction between ℃ for 1h;

[0061] (4) Add 3.38g of sodium ethylenediaminoethanesulfonate to the above s...

Embodiment 3

[0063] (1), under the protection of dry nitrogen, 40g of polyoxypropylene diol (N-220) with a number average molecular weight of 2000 and a hydroxyl value of 0.98mmol / g after vacuum dehydration, and 22.2g of isophorone isocyanate (IPDI) Add it into the reaction container, and control it at 85°C-100°C under mechanical stirring for 2h;

[0064] (2) Lower the system temperature to 40°C-60°C, add 2.05g of diethylene glycol (DEG), then add 5mL of acetone and catalyst dibutyltin dilaurate (T-12) 0.03-0.05g (3 drops ), stannous octoate (T-9) 0.03-0.05g (3 drops), under mechanical stirring, control the temperature at 55°C to 75°C for 2h;

[0065] (3) Reduce the temperature of the system to below 60°C, add 3.11g of cationic chain extender N-methyldiethanolamine (DB), and add 15mL of acetone to prevent gelation caused by excessive viscosity, and control the temperature at 40-60°C Reaction between ℃ for 1h;

[0066] (4) Add 4.35g of sodium ethylenediaminoethanesulfonate to the above sy...

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Abstract

The invention relates to a preparation method of sulfonate amphoteric polyurethane emulsion, comprising the following steps: adding oligomer polyalcohol subject to vacuum dehydration and isocyanate into a reactor under the protection of dry nitrogen, mechanically stirring the oligomer polyalcohol and the isocyanate to react for 2h at 85-100 DEG C, reducing the system temperature to 40-60 DEG C, adding a micro-molecule chain extender, a solvent, a catalyst stannous octoate (T-9) and dibutyltin dilaurate (T-12), and maintaining the temperature to react for 2h at 55-75 DEG C; reducing the systemtemperature below 60 DEG C, and adding a positive ion chain extender and the solvent to control the temperature between 40 DEG C and 60 DEG C to react for 1h; adding the sulfonate and the solvent; adding water to carry out emulsion dispersion until the content of an isocyanate group can not change in a generated prepolymer to be reacted; and decompressing, distilling and desolventizing to obtain the sulfonate amphoteric polyurethane emulsion. The prepared sulfonate amphoteric polyurethane emulsion has a certain acidity-alkalinity resistance and can be used as an excellent carrier of a biological macromolecule and a more ideal protein model compound.

Description

technical field [0001] The invention relates to a preparation method of a polymer material, in particular to an amphoteric polyurethane emulsion containing sulfonate groups and tertiary amino groups in the molecular chain. Background technique [0002] At present, there are few reports on amphoteric polyurethanes, and these reports are all amphoteric polyurethanes based on dihydroxymethylpropionic acid (DMPA) and tertiary amino groups. Due to the characteristics of dihydroxymethylpropionic acid (DMPA), this type of polyurethane is mainly There are the following disadvantages: A. The reaction time is long, generally about 8 hours from raw materials to products; B. Continuous production is difficult, and DMPA is used as a hydrophilic chain extender, and the prepolymer material must be transferred from the reactor to the emulsification The emulsion is prepared by high-speed shear emulsification and dispersion in the barrel, and then returned to the still for desolventization; C...

Claims

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Application Information

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IPC IPC(8): C08G18/10C08G18/48C08G18/42C08G18/75
Inventor 许戈文王萃萃熊潜生鲍俊杰张彪
Owner ANHUI UNIVERSITY
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