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Organosilicone modified isocyanate prepolymer for solvent-free type synthetic leather and preparation method thereof

A technology of isocyanate prepolymerization and synthetic leather, which is applied in textiles and papermaking, etc. It can solve problems such as long curing time, inability to solve solvent pollution, and unsatisfactory air and moisture permeability, and achieve excellent flexibility, air permeability, and excellent hand feeling The effect of flexibility, excellent moisture permeability and air permeability

Active Publication Date: 2018-04-20
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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  • Organosilicone modified isocyanate prepolymer for solvent-free type synthetic leather and preparation method thereof
  • Organosilicone modified isocyanate prepolymer for solvent-free type synthetic leather and preparation method thereof
  • Organosilicone modified isocyanate prepolymer for solvent-free type synthetic leather and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Weigh 100g of octamethylcyclotetrasiloxane and 61g of tetramethyltetraphenylcyclotetrasiloxane into a three-necked flask with a thermometer and a reflux device, N 2 Protect, warm up to 60℃, add 4.83g concentrated sulfuric acid, stir and react for 30min, add 7.5g tetramethyldihydrodisiloxane, stir and react at 60℃ for 5h, after the reaction, cool to room temperature, use carbonic acid Sodium hydrogen neutralizes the reaction solution to neutrality, washes with water, filters, and uses a rotary evaporator at 130°C to remove small molecular by-products, rotary evaporates for 4 hours, and filtered under reduced pressure to obtain a hydrogen end seal with a number average molecular weight of 3000 End methyl phenyl polysiloxane.

[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 The catalyst was reacted for 4h to prepare the amino...

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 and react for 40min. Then 11.3g of tetramethyldihydrodisiloxane was added, and the reaction was stirred at 80℃ for 5h. After the reaction, the temperature was lowered to room temperature, neutralized with sodium oxycarbonate to neutrality, washed with water, filtered, and heated at 130 with a rotary evaporator. The small molecule by-products were removed by rotary evaporation at ℃, rotary evaporation for 4 hours, and vacuum filtration to prepare a hydrogen-terminated methylphenyl polysiloxane with a number average molecular weight of 2000.

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

Embodiment 3

[0030] (1) Weigh 100g octamethylcyclotetrasiloxane and 46g tetramethyltetraphenylcyclotetrasiloxane into the reactor, heat up to 75℃, add 4.38g concentrated sulfuric acid, stir and react for 30min, then add 22.6g tetramethyldihydrodisiloxane, stirred at 75℃ for 5h, after the reaction, cooled to room temperature, neutralized with sodium bicarbonate to neutrality, washed with water, filtered, and used a rotary evaporator at 130℃ Rotary steaming to remove small molecular by-products, rotating steaming for 4 hours, and filtering under reduced pressure to prepare a hydrogen-terminated methylphenyl polysiloxane with a number average molecular weight of 1000.

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

[0032] (3) First, heat the amino-terminated methylphenyl polysiloxane obtained in step 2 to 120...

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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, and specifically relates 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 artificial leather produced with PU resin and base fabric. 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 fully recovered at present. , Which not only pollutes the environment, but also causes physical damage to employees, and also affects product quality. With the increasing environmental protection pressure faced by solvent-based polyurethane synthetic leather, the development of a greener polyurethane synthetic leather method is imminent. [0003] Solvent...

Claims

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Application Information

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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
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