Method for preparing epoxy crosslinking agent

Abstract

The present invention relates to the preparation method of epoxy-based crosslinking agent, comprising the following steps: (1) synthesis and purification of polyethylene glycol-polyester, (2) polyethylene glycol-polyester, epichlorohydrin and benzyl Triethylammonium chloride is mixed to prepare a light yellow transparent liquid product; the obtained product is used to prepare degradable materials, especially tissue engineering scaffold materials, and different degradation rates and mechanical strengths can be adjusted by adjusting the molecular weight and dosage of crosslinking agents. Make the degradation rate of the material match the rate of tissue formation; the degradation products of the material are non-toxic to cells and will not have adverse effects on the tissue; the cell affinity of the material surface can promote the adsorption of tissue cells on the material surface.

Description

technical field

[0001] The invention also relates to a preparation method of the epoxy-based crosslinking agent. Background technique

[0002] Biodegradable materials mainly include biodegradable films and biodegradable scaffold materials. At present, almost all degradable materials such as photodegradable materials studied at home and abroad are made of polyethylene as the matrix material through appropriate modification, and its residual film will cause harm to crops and water resources if it remains in the soil for a long time. If the photosensitive group is introduced into the polymer chain, the pollution problem of degradation products will be better solved, but it is also difficult to popularize due to problems such as processing and production. As a naturally degradable material, biodegradable materials play a unique role in environmental protection, and their application and development have been rapidly developed. There are mainly three types of biodegradable mate...

Examples

Embodiment 1

[0023] 13.5g of lactide, 6g of PEG400 and 0.17g of stannous octoate were mixed and stirred, blown with nitrogen, heated to 130°C, and reacted for 6 hours. The crude product was dissolved in chloroform, filtered and dissolved in n-hexane, separated into layers, filtered again, and repeated several times until the liquid was completely transparent, and then dried under vacuum at 55°C for one day. Take 5g of the product, 7.5g of epichlorohydrin and 0.15g of benzyltriethylammonium chloride, add 4g of 50% sodium hydroxide dropwise for 30min under stirring at room temperature, then stir and react at 60°C for 1h; cool, filter with suction, and separate the liquids The organic layer was separated, washed three times with 60 ml of saturated brine, dried over anhydrous magnesium sulfate, and distilled under reduced pressure to obtain a light yellow transparent liquid.

Embodiment 2

[0025] 15g of lactide, 2g of glycerin and 0.15g of stannous octoate were mixed and stirred, nitrogen was blown, the temperature was raised to 130°C, and the reaction was carried out for 6 hours. The crude product was dissolved in chloroform, filtered and dissolved in n-hexane, separated into layers, filtered again, and repeated several times until the liquid was completely transparent, and then dried under vacuum at 55°C for one day. Take 5g of the product, 5g of epichlorohydrin and 0.3g of benzyltriethylammonium chloride, add 3g of 50% sodium hydroxide dropwise for 30min under stirring at room temperature, then stir and react at 60°C for 1h; The organic layer was taken out, washed three times with 60 ml of saturated brine, dried over anhydrous magnesium sulfate, and distilled under reduced pressure to obtain a light yellow transparent liquid.

Embodiment 3

[0027] Mix and stir 12g of lactide, 6g of PEG800 and 0.15g of stannous octoate, blow nitrogen, raise the temperature to 130°C, and react for 6 hours. The crude product was dissolved in chloroform, filtered and dissolved in n-hexane, separated into layers, filtered again, and repeated several times until the liquid was completely transparent, and then dried under vacuum at 55°C for one day. Take 5g of the product, 5g of epichlorohydrin and 0.15g of benzyltriethylammonium chloride, add 4g of 50% sodium hydroxide dropwise for 30min under stirring at room temperature, then stir and react at 60°C for 1h; The organic layer was taken out, washed three times with 60 ml of saturated brine, dried over anhydrous magnesium sulfate, and distilled under reduced pressure to obtain a light yellow transparent liquid.

technical field

[0001] The invention also relates to a preparation method of the epoxy-based crosslinking agent. Background technique

[0002] Biodegradable materials mainly include biodegradable films and biodegradable scaffold materials. At present, almost all degradable materials such as photodegradable materials studied at home and abroad are made of polyethylene as the matrix material through appropriate modification, and its residual film will cause harm to crops and water resources if it remains in the soil for a long time. If the photosensitive group is introduced into the polymer chain, the pollution problem of degradation products will be better solved, but it is also difficult to popularize due to problems such as processing and production. As a naturally degradable material, biodegradable materials play a unique role in environmental protection, and their application and development have been rapidly developed. There are mainly three types of biodegradable mate...

Examples

Embodiment 1

[0023] 13.5g of lactide, 6g of PEG400 and 0.17g of stannous octoate were mixed and stirred, blown with nitrogen, heated to 130°C, and reacted for 6 hours. The crude product was dissolved in chloroform, filtered and dissolved in n-hexane, separated into layers, filtered again, and repeated several times until the liquid was completely transparent, and then dried under vacuum at 55°C for one day. Take 5g of the product, 7.5g of epichlorohydrin and 0.15g of benzyltriethylammonium chloride, add 4g of 50% sodium hydroxide dropwise for 30min under stirring at room temperature, then stir and react at 60°C for 1h; cool, filter with suction, and separate the liquids The organic layer was separated, washed three times with 60 ml of saturated brine, dried over anhydrous magnesium sulfate, and distilled under reduced pressure to obtain a light yellow transparent liquid.

Embodiment 2

[0025] 15g of lactide, 2g of glycerin and 0.15g of stannous octoate were mixed and stirred, nitrogen was blown, the temperature was raised to 130°C, and the reaction was carried out for 6 hours. The crude product was dissolved in chloroform, filtered and dissolved in n-hexane, separated into layers, filtered again, and repeated several times until the liquid was completely transparent, and then dried under vacuum at 55°C for one day. Take 5g of the product, 5g of epichlorohydrin and 0.3g of benzyltriethylammonium chloride, add 3g of 50% sodium hydroxide dropwise for 30min under stirring at room temperature, then stir and react at 60°C for 1h; The organic layer was taken out, washed three times with 60 ml of saturated brine, dried over anhydrous magnesium sulfate, and distilled under reduced pressure to obtain a light yellow transparent liquid.

Embodiment 3

[0027] Mix and stir 12g of lactide, 6g of PEG800 and 0.15g of stannous octoate, blow nitrogen, raise the temperature to 130°C, and react for 6 hours. The crude product was dissolved in chloroform, filtered and dissolved in n-hexane, separated into layers, filtered again, and repeated several times until the liquid was completely transparent, and then dried under vacuum at 55°C for one day. Take 5g of the product, 5g of epichlorohydrin and 0.15g of benzyltriethylammonium chloride, add 4g of 50% sodium hydroxide dropwise for 30min under stirring at room temperature, then stir and react at 60°C for 1h; The organic layer was taken out, washed three times with 60 ml of saturated brine, dried over anhydrous magnesium sulfate, and distilled under reduced pressure to obtain a light yellow transparent liquid.

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