Preparation method of compound emulsifier in-situ crosslinking chitosan quaternary ammonium salt essential oil microcapsule

Abstract

The invention discloses a preparation method of a compound emulsifier in-situ crosslinking chitosan quaternary ammonium salt essential oil microcapsule. A compound emulsifier which has the dual functions of an emulsifier and a cross-linking agent is prepared through double hydroformylation modification on polyethylene glycol; in the preparation process of the chitosan quaternary ammonium salt essential oil microcapsule, on one hand, essential oil is emulsified by a polyethylene glycol long carbon chain structure in the compound emulsifier, on the other hand, chitosan quaternary ammonium salt crosslinking is conducted through a condensation reaction between aldehyde groups at the two ends of the compound emulsifier and amino groups on the chitosan quaternary ammonium salt, and then synchronization of the essential oil emulsifying process and the chitosan quaternary ammonium salt crosslinking process is achieved. According to the preparation method, by grafting aldehyde molecules achieving the chitosan quaternary ammonium salt crosslinking function onto polyethylene glycol, freeing of micromolecular aldehyde in the essential oil microcapsule preparation process is avoided, therefore, the content of micromolecular aldehyde in the essential oil microcapsule product is decreased, and the toxicity of the product is lowered.

Description

technical field

[0001] The invention belongs to the technical field of textile finishing, and specifically relates to a method for preparing chitosan quaternary ammonium salt essential oil microcapsules with chitosan quaternary ammonium salt as a wall material and essential oil as a core material by in-situ crosslinking of a composite emulsifier. Background technique

[0002] With the development of the economy and the improvement of living standards, people's requirements for textiles have undergone great changes. From the past practical type to the decoration, enjoyment, and health care type, textile perfuming conforms to this trend. Because scented textiles have the functions of antibacterial and insect repellent, masking peculiar smell, and making body and mind comfortable, people generally like the combination of fragrance and textiles for a long time. In ancient my country, there was a habit of sewing sachets on clothes; Since the Middle Ages, spraying perfume on clothe...

Examples

preparation example Construction

[0018] The preparation method of composite emulsifier in-situ cross-linked chitosan quaternary ammonium salt essential oil microcapsules of the present invention comprises the following steps:

[0019] (1) Preparation of compound emulsifier

[0020] Add 20~40 parts of polyethylene glycol, 30~60 parts of anhydrous dimethyl sulfoxide, 10~20 parts of chloroform into the reaction bottle, after ultrasonic dissolution, add 25~50 parts of acetic anhydride, and under the condition of magnetic stirring Stir and react at room temperature for 12-16 hours to complete the double aldehyde modification of polyethylene glycol, and then remove dimethyl sulfoxide by distillation under reduced pressure to obtain a composite emulsifier;

[0021] (2) Preparation of chitosan quaternary ammonium salt essential oil microcapsules

[0022] Weigh 3.4~13.4 parts of chitosan quaternary ammonium salt into the reaction flask, then add 0.2~0.8 parts of compound emulsifier prepared in step (1), 10~40 parts o...

Embodiment 1

[0026] Add 20 parts of polyethylene glycol with a molecular weight of 200, 30 parts of anhydrous dimethyl sulfoxide, and 10 parts of chloroform into the reaction bottle, ultrasonically until it is completely dissolved, then add 25 parts of acetic anhydride, and fix the three-necked flask on the iron stand. Stir magnetically, react at room temperature for 12 hours, heat in a water bath at 60°C and distill under reduced pressure (to remove dimethyl sulfoxide) to obtain bisaldehydelated polyethylene glycol. Weigh the molecular weight as 1×10 5 3.4 parts of chitosan quaternary ammonium salt with an oxygen substitution degree of 65%, 0.2 parts of polyoxyethylene glycol, 10 parts of lemongrass essential oil or clove oil, and 86.4 parts of deionized water are added to the reaction bottle, and the reaction bottle is fixed On an iron stand with mechanical stirring, carry out emulsification for 30 minutes with a mechanical stirring speed of 1000 rpm / min, after emulsification, adjust the...

Embodiment 2

[0028] Add 40 parts of polyethylene glycol with a molecular weight of 1000, 60 parts of anhydrous dimethyl sulfoxide, and 20 parts of chloroform into the reaction flask, sonicate until completely dissolved, then add 25 parts of acetic anhydride, stir at room temperature for 14 hours, and depressurize at 65°C Distillation (removal of dimethylsulfoxide) yields bisaldehydelated polyethylene glycol. Weigh the molecular weight as 2×10 5 6.7 parts of chitosan quaternary ammonium salt with an oxygen substitution degree of 65%, 0.4 parts of polyoxyethylene glycol, 20 parts of lemongrass essential oil or clove oil, 72.9 parts of deionized water, emulsified for 50 minutes, and the mechanical stirring speed is 1000rpm / min , after emulsification, adjust the mechanical stirring speed to 600rpm / min, react at 25°C for 5h, and at 45°C for 2h, after the reaction, use 30% NaOH aqueous solution to adjust the pH to 9, and then After reacting for 1 hour, filtering, washing and drying, the chitosa...

technical field

[0001] The invention belongs to the technical field of textile finishing, and specifically relates to a method for preparing chitosan quaternary ammonium salt essential oil microcapsules with chitosan quaternary ammonium salt as a wall material and essential oil as a core material by in-situ crosslinking of a composite emulsifier. Background technique

[0002] With the development of the economy and the improvement of living standards, people's requirements for textiles have undergone great changes. From the past practical type to the decoration, enjoyment, and health care type, textile perfuming conforms to this trend. Because scented textiles have the functions of antibacterial and insect repellent, masking peculiar smell, and making body and mind comfortable, people generally like the combination of fragrance and textiles for a long time. In ancient my country, there was a habit of sewing sachets on clothes; Since the Middle Ages, spraying perfume on clothe...

Examples

preparation example Construction

[0018] The preparation method of composite emulsifier in-situ cross-linked chitosan quaternary ammonium salt essential oil microcapsules of the present invention comprises the following steps:

[0019] (1) Preparation of compound emulsifier

[0020] Add 20~40 parts of polyethylene glycol, 30~60 parts of anhydrous dimethyl sulfoxide, 10~20 parts of chloroform into the reaction bottle, after ultrasonic dissolution, add 25~50 parts of acetic anhydride, and under the condition of magnetic stirring Stir and react at room temperature for 12-16 hours to complete the double aldehyde modification of polyethylene glycol, and then remove dimethyl sulfoxide by distillation under reduced pressure to obtain a composite emulsifier;

[0021] (2) Preparation of chitosan quaternary ammonium salt essential oil microcapsules

[0022] Weigh 3.4~13.4 parts of chitosan quaternary ammonium salt into the reaction flask, then add 0.2~0.8 parts of compound emulsifier prepared in step (1), 10~40 parts o...

Embodiment 1

[0026] Add 20 parts of polyethylene glycol with a molecular weight of 200, 30 parts of anhydrous dimethyl sulfoxide, and 10 parts of chloroform into the reaction bottle, ultrasonically until it is completely dissolved, then add 25 parts of acetic anhydride, and fix the three-necked flask on the iron stand. Stir magnetically, react at room temperature for 12 hours, heat in a water bath at 60°C and distill under reduced pressure (to remove dimethyl sulfoxide) to obtain bisaldehydelated polyethylene glycol. Weigh the molecular weight as 1×10 5 3.4 parts of chitosan quaternary ammonium salt with an oxygen substitution degree of 65%, 0.2 parts of polyoxyethylene glycol, 10 parts of lemongrass essential oil or clove oil, and 86.4 parts of deionized water are added to the reaction bottle, and the reaction bottle is fixed On an iron stand with mechanical stirring, carry out emulsification for 30 minutes with a mechanical stirring speed of 1000 rpm / min, after emulsification, adjust the...

Embodiment 2

[0028] Add 40 parts of polyethylene glycol with a molecular weight of 1000, 60 parts of anhydrous dimethyl sulfoxide, and 20 parts of chloroform into the reaction flask, sonicate until completely dissolved, then add 25 parts of acetic anhydride, stir at room temperature for 14 hours, and depressurize at 65°C Distillation (removal of dimethylsulfoxide) yields bisaldehydelated polyethylene glycol. Weigh the molecular weight as 2×10 5 6.7 parts of chitosan quaternary ammonium salt with an oxygen substitution degree of 65%, 0.4 parts of polyoxyethylene glycol, 20 parts of lemongrass essential oil or clove oil, 72.9 parts of deionized water, emulsified for 50 minutes, and the mechanical stirring speed is 1000rpm / min , after emulsification, adjust the mechanical stirring speed to 600rpm / min, react at 25°C for 5h, and at 45°C for 2h, after the reaction, use 30% NaOH aqueous solution to adjust the pH to 9, and then After reacting for 1 hour, filtering, washing and drying, the chitosa...