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A kind of silicone-modified isocyanate prepolymer for solvent-free synthetic leather and preparation method thereof

A technology of isocyanate prepolymerization and synthetic leather, which is applied in the direction of textiles and paper making, can solve the problems of long curing time, unsatisfactory air and moisture permeability, and inability to solve solvent pollution, etc., and achieve excellent flexibility and air permeability, excellent air permeability Moisture breathability, excellent hand softness effect

Active Publication Date: 2021-02-09
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent document CN 106087451A discloses a preparation method of breathable synthetic leather, by preparing polyether amino silicone oil modified polyurethane, then adding additives, coating, solidifying, washing and drying to prepare breathable polyurethane synthetic leather, but the water consumption in the preparation process Large, it takes 2-3 hours to wash, dry and cure, and the curing time is long. This method has the disadvantages of polluting the environment and low production efficiency. The air permeability of the prepared synthetic leather can reach 725ml / cm 2 h, the moisture permeability is 962g / m 2 24 hours
Patent document CN104558494 A discloses a highly moisture-permeable modified polyurethane and its preparation method to prepare a synthetic leather surface layer resin, which solves the phase separation problem of dihydroxyalkyl polysiloxane and polyether polyol by pre-polymerization treatment. However, the preparation of silicone-modified polyurethane still requires the use of a large amount of organic solvents, which cannot solve the problem of solvent pollution
[0005] Although the above method can improve or change some properties of polyurethane by modifying polyurethane with silicone, there are still disadvantages such as not being conducive to environmental protection, and the air and moisture permeability cannot meet the requirements.

Method used

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  • A kind of silicone-modified isocyanate prepolymer for solvent-free synthetic leather and preparation method thereof
  • A kind of silicone-modified isocyanate prepolymer for solvent-free synthetic leather and preparation method thereof
  • A kind of silicone-modified isocyanate prepolymer for solvent-free synthetic leather and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Take by weighing 100g octamethylcyclotetrasiloxane and 61g tetramethyltetraphenylcyclotetrasiloxane and join in the there-necked flask with thermometer and condensation reflux device, N 2 protection, raised the temperature to 60°C, then added 4.83g of concentrated sulfuric acid, stirred for 30min, then added 7.5g of tetramethyldihydrodisiloxane, and stirred for 5h at 60°C. Sodium hydrogen neutralizes the reaction solution to neutrality, washes with water, filters, uses a rotary evaporator at 130°C to remove small molecule by-products, rotates for 4 hours, and filters under reduced pressure to obtain a hydrogen-terminated group-sealed product with a number average molecular weight of 3000. terminal methylphenylpolysiloxane.

[0023] (2) Weigh 100g of the hydrogen-terminated methylphenyl polysiloxane obtained in step (1) and 3.8g of allylamine into the reactor, raise the temperature to 50°C, and add 0.001g of H 2 PtCl 6 Catalyst, reacted for 4h to prepare amino-term...

Embodiment 2

[0026] (1) Weigh 100g of octamethylcyclotetrasiloxane and 57.5g of tetramethyltetraphenylcyclotetrasiloxane into the reactor, raise the temperature to 80°C, add 3.15g of concentrated sulfuric acid, and stir for 40min. Then add 11.3g of tetramethyldihydrodisiloxane, stir and react at 80°C for 5h. Rotary evaporation at ℃ to remove small molecular by-products, rotary evaporation for 4 hours, and filtration under reduced pressure to prepare a hydrogen-terminated methylphenyl polysiloxane with a number average molecular weight of 2000.

[0027] (2) Weigh 100g of hydrogen-terminated methylphenylpolysiloxane and 5.7g of allylamine into the reactor, raise the temperature to 60°C, and add 0.002g of H 2 PtCl 6 Catalyst, reacted for 4h to prepare amino-terminated methylphenylpolysiloxane.

[0028] (3) The amino-terminated methylphenyl polysiloxane obtained in the step (2) is dehydrated at room temperature to 120° C. for 4 hours under reduced pressure, and then used. Add 100g of isopho...

Embodiment 3

[0030] (1) Weigh 100g of octamethylcyclotetrasiloxane and 46g of tetramethyltetraphenylcyclotetrasiloxane into the reactor, raise the temperature to 75°C, add 4.38g of concentrated sulfuric acid, stir for 30min, then add 22.6g of tetramethyldihydrodisiloxane, stirred and reacted at 75°C for 5h, after the reaction, cooled to room temperature, neutralized to neutral with sodium bicarbonate, washed with water, filtered, and heated at 130°C with a rotary evaporator Rotary evaporation removed small molecular by-products, rotary evaporation for 4 hours, and filtration under reduced pressure to prepare a hydrogen-terminated methylphenylpolysiloxane with a number average molecular weight of 1000.

[0031] (2) Weigh 100g of hydrogen-terminated methylphenyl polysiloxane and 7.6g of allylamine into the reactor, heat up to 60°C, add 0.003g of H 2 PtCl 6 Catalyst, reacted for 4h to prepare amino-terminated methylphenylpolysiloxane.

[0032] (3) First heat the amino-terminated methylpheny...

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Abstract

The invention discloses an organosilicone modified isocyanate prepolymer for solvent-free type synthetic leather and a preparation method thereof. The prepolymer contains a compound in the structure shown in the description, wherein R is aryl or fatty group; a and b are natural numbers. The preparation method comprises the following steps that (1) octamethylcyclotetrasiloxane, 2,4,6,8-tetramethyl-2,4,6,8-tetraphenylcyclotetrasiloxane and acid catalysts are added into a reactor; then, tetramethyl dihydrodisiloxane is added; ring-opening polymerization reaction is performed for 4 to 6h at 60 to80 DEG C; temperature reduction, neutralization, water washing, filtering and micromolecule by-product removal are performed to obtain hydrogen-terminated blocking methyl phenyl polysiloxane; (2) thehydrogen-terminated methyl phenyl polysiloxane obtained in the step (1) and allyl amine react under H2PtCl6 catalysts to prepare hydrogen-terminated blocking methyl phenyl polysiloxane; (3) the product in the step (2) is dehydrated and then reacts with isocyanate monomers to generate the prepolymer with the terminal group being NCO.

Description

technical field [0001] The invention belongs to the field of solvent-free synthetic leather, in particular to an organosilicon-modified isocyanate prepolymer for preparing solvent-free synthetic leather and a preparation method thereof. Background technique [0002] Polyurethane (PU) synthetic leather is an artificial leather produced with PU resin and base cloth. Traditional synthetic leather is mainly solvent-based synthetic leather, and its solvents are mostly organic solvents such as dimethylformamide, toluene and acetone with low boiling points and volatiles. These solvents account for 70% to 80%, and they cannot be completely recovered at present. , not only pollute the environment, but also cause physical damage to employees, and also affect product quality. With the increase of environmental protection pressure faced by solvent-based polyurethane synthetic leather, it is imminent to develop greener polyurethane synthetic leather methods. [0003] Solvent-free polyu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/61C08G18/10C08L75/04D06N3/00D06N3/14
CPCC08G18/10C08G18/61C08L75/04D06N3/0045D06N3/0077D06N3/142D06N3/147
Inventor 温荣政董火成赵修文曹敏孙嘉鹏李宁
Owner LIMING RES INST OF CHEM IND