Soft sheet and preparation method thereof

Abstract

The invention belongs to the technical field of textile auxiliaries, and particularly discloses a film and a preparation method thereof.The film is prepared from, by mass, 100-120 parts of hydrogenated palm oil; 15 to 30 parts of ethanolamine; 1 to 3 parts of dicyclohexylcarbodiimide; 25 to 40 parts of hexamethylene diisocyanate; 10 to 30 parts of single-terminated hydroxyl methyl silicone oil; 2 to 5 parts of dimethyl sulfate; 5-15 parts of an emulsifier; and 5-10 parts of glacial acetic acid. By adopting the soft sheet and the preparation method thereof, the problems of harsh reaction conditions, poor product uniformity, single hand feeling and low use safety of the soft sheet in the prior art are solved.

Description

Technical Field

[0001] The invention relates to the technical field of textile printing and dyeing auxiliaries, in particular to a soft film and a preparation method thereof. Background Art

[0002] During the dyeing and finishing process, the fiber is easily damaged in various processing steps, which leads to a rough feel of the fiber; at the same time, the fiber will lose its feel after various resin finishing, so softeners must be added for finishing to obtain a soft and fluffy feel. The softeners mainly used in the industry include soft film and silicone oil. Soft film can not only give the fiber a different style and feel, but also improve the dyeing and finishing process, save energy, and reduce processing costs; soft film has the characteristics of simple packaging, small size, easy storage and transportation, and low cost, so it is very popular in printing and dyeing factories.

[0003] The existing films on the market are mainly obtained by the synthesis reaction of stearic acid and diethylenetriamine or hydroxyethylethylenediamine. Since the reaction of stearic acid and diethylenetriamine adopts the traditional high-temperature amidation reaction, the product structure is complex and multiple mixtures exist at the same time, so the uniformity of product performance is poor. At the same time, the high-temperature reaction is poorly controllable, which easily causes differences in the uniformity of product appearance; and hydroxyethylethylenediamine will have adverse effects on fetal development after long-term contact. Therefore, the uniformity and safety of films are long-term difficulties that the industry needs to solve. Summary of the invention

[0004] The purpose of the present invention is to provide a film and a preparation method thereof, so as to solve the problems of harsh reaction conditions, poor product uniformity, single feel and safety in use of the prior art films.

[0005] To achieve the above object, the present invention provides a film comprising the following raw materials in parts by weight: 100-120 parts of hydrogenated palm oil; 15-30 parts of ethanolamine; 1-3 parts of dicyclohexylcarbodiimide; Hexamethylene diisocyanate 25-40 parts; 10-30 parts of mono-terminated hydroxymethyl silicone oil; 2-5 parts of dimethyl sulfate; Emulsifier 5-15 parts; 5-10 parts of glacial acetic acid.

[0006] Preferably, the relative molecular mass of the single-end hydroxymethyl silicone oil is 1900-2100.

[0007] Preferably, the emulsifier is at least one of fatty alcohol polyoxyethylene ether AEO-7 and fatty alcohol polyoxyethylene ether AEO-9.

[0008] Preferably, the mass concentration of the glacial acetic acid is not less than 98%.

[0009] A method for preparing a film comprises the following steps: S1. Melt the weighed hydrogenated palm oil by gradually heating it to 40°C at 1°C / min under nitrogen protection; S2, adding weighed ethanolamine and dicyclohexylcarbodiimide to the melted hydrogenated palm oil, gradually heating to 80-100°C at 0.5-1°C / min, maintaining a vacuum degree of 0.3-0.5MPa, and keeping the temperature for 2-4 hours until no water is produced to obtain a primary product; S3, cooling the above-mentioned initial product to 60-70° C., adding weighed single-end hydroxymethyl silicone oil and hexamethylene diisocyanate, and keeping the temperature for reaction for 1-3 hours to obtain an intermediate product; S4, raising the temperature of the intermediate product to 80-100° C., adding weighed dimethyl sulfate, keeping the temperature for reaction for 1-3 hours, adding weighed emulsifier and glacial acetic acid, keeping the temperature for another 1-2 hours, discharging the product, and slicing to obtain a film.

[0010] The advantages and beneficial effects of the present invention using the above-mentioned film and preparation method thereof are: 1. The product structure of the present invention simultaneously introduces long carbon chains and long chain silane structures, thereby giving the product excellent fluffy and soft properties.

[0011] 2. The product of the present invention has mild reaction conditions and excellent uniformity of product appearance.

[0012] 3. The present invention selects hexamethylene diisocyanate, and the polycondensation reaction has obvious selectivity, good reaction controllability, clear product structure, few by-products, and good uniformity of product performance.

[0013] 4. The raw materials selected in the present invention have good biocompatibility, so the product safety is excellent.

[0014] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a flow chart of the film preparation method of the present invention. DETAILED DESCRIPTION

[0016] The technical solution of the present invention is further described below through the accompanying drawings and embodiments.

[0017] Unless otherwise defined, technical or scientific terms used in the present invention shall have the common meanings understood by one having ordinary skills in the field to which the present invention belongs.

[0018] Unless otherwise defined, the reagents and equipment used in the present invention are commonly available from the market.

[0019] A film comprising the following raw materials in parts by weight: 100-120 parts of hydrogenated palm oil; 15-30 parts of ethanolamine; 1-3 parts of dicyclohexylcarbodiimide; Hexamethylene diisocyanate 25-40 parts; 10-30 parts of single-end hydroxymethyl silicone oil, the relative molecular mass of the single-end hydroxymethyl silicone oil is 1900-2100; 2-5 parts of dimethyl sulfate; 5-15 parts of an emulsifier, wherein the emulsifier is at least one of fatty alcohol polyoxyethylene ether AEO-7 and fatty alcohol polyoxyethylene ether AEO-9; 5-10 parts of glacial acetic acid, the mass concentration of glacial acetic acid is not less than 98%.

[0020] A method for preparing a film comprises the following steps: S1. Melt the weighed hydrogenated palm oil by gradually heating it to 40°C at 1°C / min under nitrogen protection; S2, adding weighed ethanolamine and dicyclohexylcarbodiimide to the melted hydrogenated palm oil, gradually heating to 80-100°C at 0.5-1°C / min, maintaining a vacuum degree of 0.3-0.5MPa, and keeping the temperature for 2-4 hours until no water is produced to obtain a primary product; S3, cooling the above-mentioned initial product to 60-70° C., adding weighed single-end hydroxymethyl silicone oil and hexamethylene diisocyanate, and keeping the temperature for reaction for 1-3 hours to obtain an intermediate product; S4, raising the temperature of the intermediate product to 80-100° C., adding weighed dimethyl sulfate, keeping the temperature for reaction for 1-3 hours, adding weighed emulsifier and glacial acetic acid, keeping the temperature for another 1-2 hours, discharging the product, and slicing to obtain a film.

[0021] Example 1 A method for preparing a film comprises the following steps: 1. Melt 100g hydrogenated palm oil by gradually heating to 40℃ at 1℃ / min under nitrogen protection; 2. Add 15g of ethanolamine and 1g of dicyclohexylcarbodiimide to the melted hydrogenated palm oil, gradually raise the temperature to 80°C at 0.5°C / min, maintain the vacuum degree at 0.3MPa, and keep the temperature for 2 hours until no water is produced to obtain the primary product; 3. Cool the above-mentioned initial product to 60°C, add 10g of single-end hydroxymethyl silicone oil and 25g of hexamethylene diisocyanate, and keep the temperature to react for 1 hour to obtain an intermediate product; 4. Heat the intermediate product to 80°C, add 2g of dimethyl sulfate, keep warm for 1 hour, add 5g of fatty alcohol polyoxyethylene ether AEO-7 and 5g of glacial acetic acid, keep warm for 1 hour, discharge the material, and slice to obtain a film.

[0022] Example 2 A method for preparing a film comprises the following steps: 1. Melt 120g hydrogenated palm oil by gradually heating to 40℃ at 1℃ / min under nitrogen protection; 2. Add 30 g of ethanolamine and 3 g of dicyclohexylcarbodiimide to the melted hydrogenated palm oil, gradually raise the temperature to 100 °C at 1 °C / min, maintain the vacuum degree at 0.5 MPa, and keep the temperature for 4 hours until no water is produced to obtain the primary product; 3. Cool the above-mentioned initial product to 70°C, add 30g of single-end hydroxymethyl silicone oil and 40g of hexamethylene diisocyanate, and keep the temperature to react for 3 hours to obtain an intermediate product; 4. Heat the intermediate product to 100°C, add 5g of dimethyl sulfate, keep warm for 3 hours, add 15g of fatty alcohol polyoxyethylene ether AEO-9 and 10g of glacial acetic acid, keep warm for 2 hours, discharge the material, and slice to obtain a film.

[0023] Example 3 A method for preparing a film comprises the following steps: 1. Melt 110g hydrogenated palm oil by gradually heating to 40℃ at 1℃ / min under nitrogen protection; 2. Add 23g of ethanolamine and 2g of dicyclohexylcarbodiimide to the melted hydrogenated palm oil, gradually raise the temperature to 90°C at 0.8°C / min, maintain the vacuum degree at 0.4MPa, and keep the reaction for 3 hours until no water is produced to obtain the primary product; 3. Cool the above-mentioned initial product to 65°C, add 20g of single-end hydroxymethyl silicone oil and 35g of hexamethylene diisocyanate, and keep the temperature to react for 2 hours to obtain an intermediate product; 4. Heat the intermediate product to 90°C, add 4g of dimethyl sulfate, keep warm for 2 hours, add 10g of fatty alcohol polyoxyethylene ether AEO-9 and 8g of glacial acetic acid, keep warm for 2 hours, discharge the material, and slice to obtain a film.

[0024] The film prepared in the above examples 1-3 and the comparative commercial film (the product obtained by the reaction of stearic acid and diethylenetriamine) were prepared into a 10% aqueous solution, and the aqueous solution stability was observed after standing for 1 hour; then the film was applied to the soft finishing of cotton knitted fabrics, and the cotton knitted fabrics were treated by immersion method according to 3% of the mass of the fabric sample, bath ratio 1:10, working liquid temperature 35°C, time 15 minutes, 140°C drying, and the fabric sample was left to regain moisture for 3 hours before testing the whiteness and feel. The whiteness can be tested by a whiteness meter, which can show the yellowing of the fabric sample; the feel is evaluated by a group of 5 people, with 1 being the worst and 5 being the best. The sum of the scores of the 5 people is the feel score, and the higher the score, the better the feel. The specific data is shown in Table 1.

[0025] Table 1 Performance test results of different samples

[0026] It can be seen from the data in the above table that the fabric samples treated with the film obtained in Examples 1-3 of the present invention have excellent hand feel and good fabric whiteness effect, which is due to the comprehensive effect of combining long carbon chain and long chain siloxane in the film structure of the present invention. The present invention obtains the primary product by low temperature amidation reaction of hydrogenated palm oil and ethanolamine under the catalytic action of dicyclohexylcarbodiimide, and the obtained primary product reacts with single-terminal hydroxymethyl silicone oil and hexamethylene diisocyanate at low temperature to obtain an intermediate product, and then completes quaternization under the action of dimethyl sulfate, and then adds emulsifier and glacial acetic acid to obtain a functional film. Due to the mild reaction conditions of the product, the uniformity of the product appearance is excellent; at the same time, the hexamethylene diisocyanate reaction has obvious selectivity, good reaction controllability, clear product structure, few by-products, and good uniformity of product performance; long carbon chain and long chain silane structure are introduced into the product structure at the same time, so as to give the product application excellent fluffy and soft properties; the raw materials selected by the present invention have good biocompatibility, so the product safety is excellent.

[0027] Therefore, the present invention adopts the above-mentioned soft film and the preparation method thereof, and simultaneously introduces a long carbon chain and a long-chain silane structure into the product structure, thereby giving the product excellent fluffy and soft properties; the reaction conditions are mild, and the product appearance has excellent uniformity; hexamethylene diisocyanate is selected, the polycondensation reaction has obvious selectivity, good reaction controllability, a clear product structure, few by-products, and good uniformity of product performance; the raw materials have good biocompatibility, so the product safety is excellent.

[0028] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that they can still modify or replace the technical solution of the present invention with equivalents, and these modifications or equivalent replacements cannot cause the modified technical solution to deviate from the spirit and scope of the technical solution of the present invention.

Claims

1. A film, characterized in that: The invention comprises the following raw materials in parts by weight: 100-120 parts of hydrogenated palm oil; 15-30 parts of ethanolamine; 1-3 parts of dicyclohexylcarbodiimide; 25-40 parts of hexamethylene diisocyanate; 10-30 parts of mono-terminal hydroxymethyl silicone oil; 2-5 parts of dimethyl sulfate; Emulsifier 5-15 parts; 5-10 parts of glacial acetic acid.

2. A film according to claim 1, characterized in that: The relative molecular mass of the single-end hydroxymethyl silicone oil is 1900-2100.

3. A film according to claim 1, characterized in that: The emulsifier is at least one of fatty alcohol polyoxyethylene ether AEO-7 and fatty alcohol polyoxyethylene ether AEO-9.

4. A film according to claim 1, characterized in that: The mass concentration of the glacial acetic acid is not less than 98%.

5. A method for preparing a film according to any one of claims 1 to 4, characterized in that: The steps include: S1. Melt the weighed hydrogenated palm oil by gradually heating it to 40°C at 1°C / min under nitrogen protection; S2, adding weighed ethanolamine and dicyclohexylcarbodiimide to the melted hydrogenated palm oil, gradually heating to 80-100°C at 0.5-1°C / min, maintaining a vacuum degree of 0.3-0.5MPa, and keeping the temperature for 2-4 hours until no water is produced to obtain a primary product; S3, cooling the above-mentioned initial product to 60-70° C., adding weighed single-end hydroxymethyl silicone oil and hexamethylene diisocyanate, and keeping the temperature for reaction for 1-3 hours to obtain an intermediate product; S4, raising the temperature of the intermediate product to 80-100° C., adding weighed dimethyl sulfate, keeping the temperature for reaction for 1-3 hours, adding weighed emulsifier and glacial acetic acid, keeping the temperature for another 1-2 hours, discharging the product, and slicing to obtain a film.

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