A textile auxiliary composition and a process for its preparation

The mixed fatty acid glycerides and nonionic surfactant composition prepared by esterification reaction solves the problems of biodegradability and high cost of textile auxiliaries, realizing a low-cost and environmentally friendly textile auxiliary composition and improving application effect.

CN117822313BActive Publication Date: 2026-08-25APICAL OLEOCHEMICAL(TAIXING) CO LTD
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Patent Information

Application Number
CN202311696532.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-12
Publication Date
2026-08-25
Estimated Expiration
2043-12-12

AI Technical Summary

Technical Problem

Existing textile auxiliaries suffer from poor biodegradability, high cost, and unsatisfactory application effects. In particular, petroleum-based products are prone to causing environmental pollution, and naturally derived products are prone to emulsification instability.

Method used

Using oleochemical by-products as raw materials, mixed fatty acid glycerides and nonionic surfactants are prepared through esterification reaction to form a low-cost, environmentally friendly textile auxiliary composition, comprising 60-90% mixed fatty acid glycerides and the balance nonionic surfactants.

Benefits of technology

This invention enables low-cost, high-efficiency textile auxiliary compositions, solves the problem of utilizing oil and chemical waste, reduces environmental pollution risks, and improves the biodegradability and application effects of the products.

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Abstract

The application discloses a textile auxiliary composition, comprising: 60-90% of mixed fatty acid glyceride and the balance of mixed non-ionic surfactant, wherein the mixed fatty acid glyceride comprises a mixture of triglyceride, polyglycerol triglyceride, mixed fatty acid and polyglycerol; and the mixed non-ionic surfactant comprises fatty alcohol alkoxylate, fatty acid alkoxylate, glycerol monostearate and the like. The mixed fatty acid glyceride is first put into a reaction kettle, the reaction kettle is heated to 70 DEG C, and the mixed fatty acid glyceride is melted; the fatty acid alkoxylate, the glycerol monostearate and the fatty alcohol alkoxylate are weighed in the reaction kettle in sequence, constant temperature stirring and emulsification are carried out, and the product is obtained; then the product is transferred to a granulation packaging line, weighed, packaged and stored, and the textile auxiliary composition is obtained. The application can effectively solve the problem of oil and fat chemical waste, convert low-value by-products into high-value products, realize waste recycling and sustainable production of oil and fat chemicals.
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Description

Technical Field

[0001] This application relates to the field of textile auxiliaries, specifically to a textile auxiliary composition and its preparation method. Background Technology

[0002] Currently, there are two main types of smoothing agents used in the sizing industry: petroleum-based and natural-based. Petroleum-based products, such as those using paraffin as the main raw material, are not easily biodegradable. Besides causing environmental pollution, they also create numerous inconveniences in pre-treatment and post-treatment processes, such as low capillary efficiency and the formation of wax, dye, and oil stains on the fabric surface. Naturally sourced products, on the other hand, can be completely saponified in subsequent processes, are easy to desizing and biodegrade, and do not cause environmental pollution. However, currently, domestically produced textile products using animal and vegetable oils as raw materials exhibit emulsification instability and layering, resulting in poor application effects. Furthermore, the high cost of these textile auxiliaries is due to the high price of the raw materials.

[0003] CN103911858A discloses a natural fiber textile oiling agent and its preparation method, comprising: vegetable oil: 10-20, paraffin wax: 3-8, mineral oil: 20-30, sorbitan monooleate: 10-20; fatty alcohol polyoxyethylene ether: 4-8; octylphenol polyoxyethylene ether: 4-8; fatty alcohol sulfate: 10-20; and oleic acid polyethylene glycol: 3-5. This spinning oiling agent can improve the smoothness and wettability of sized yarn, reducing friction and preventing sizing slippage; it also improves the elongation of sized yarn and the penetration of sizing, and facilitates desizing; it does not hinder the gelatinization of sizing, remains stable in the sizing medium, and does not damage the hand feel of the textile. However, the formula contains raw materials such as paraffin wax and octylphenol polyoxyethylene ether, which are not easily biodegradable, and can cause many inconveniences in pre-dyeing and post-dyeing treatments, such as low capillary efficiency and easy formation of wax spots, dye spots, and oil spots on the fabric surface. Octylphenol polyoxyethylene ether is also an environmentally unfriendly product, easily causing harm to aquatic organisms, and its use is restricted in exports. Furthermore, the raw materials used in this formulation are expensive. Currently, there are also reports in the literature of using oleochemical byproducts as raw materials to produce textile auxiliaries.

[0004] Therefore, a solution that addresses the issue of easy separation of textile auxiliaries and reduces raw material costs is urgently needed in the industry. Summary of the Invention

[0005] In view of the above shortcomings, the present invention provides a method for preparing a mixture of polymeric glycerol esters and fatty acid esters by reacting byproducts of oleochemical industry. Specifically, fatty acid byproducts and glycerol byproducts are added to a reaction vessel, an acidic catalyst is added, and the esterification reaction is carried out at 200-245°C for 5-7 hours initially with nitrogen to remove water. After the reaction is slowed down, the temperature is lowered to 160-170°C, and the reaction is carried out under vacuum until no water is carried out. The product obtained is the mixed fatty acid glycerol ester.

[0006] This invention is achieved through the following technical means:

[0007] A textile auxiliary composition comprising:

[0008] 60-90% by weight of mixed fatty acid glycerides; and

[0009] The remainder is mixed with nonionic surfactants; wherein:

[0010] The mixed fatty acid glycerides are a mixture of triglycerides, polyglycerides, mixed fatty acids, and polyglycerols obtained by esterification of oleochemical by-products.

[0011] The mixed nonionic surfactants include: 2-10 parts fatty alcohol alkoxylates, 0-6 parts fatty acid alkoxylates, and 3-10 parts glyceryl monostearate.

[0012] Furthermore, the mixed fatty acid glycerides are prepared by the following method:

[0013] (1) Add fatty acid byproducts to a reaction vessel and heat to melt them. Start stirring to obtain melted material. Then add acidic catalyst and introduce nitrogen gas.

[0014] (2) Add glycerol byproduct dropwise at a fatty acid to glycerol mass ratio of 8:1, heat the reaction until no obvious water is carried out, and then stop the nitrogen gas flow.

[0015] (3) Cool down, start the water ring pump, and evacuate until no water is carried out.

[0016] Further, the fatty acid byproducts in step (1) include:

[0017] A mixture of palmitic acid, stearic acid, and arachidic acid;

[0018] The reactor is heated to 90°C.

[0019] Further, the acid catalyst added in step (1) is 4 parts by mass of fatty acids.

[0020] Furthermore, the temperature of the heating reaction in step (2) is 200-245℃, and the reaction time is 5-7h.

[0021] Furthermore, the heating reaction temperature is 220°C, and the reaction time is 6 hours.

[0022] Further, step (3) involves cooling the temperature to 160-170°C.

[0023] The present invention also discloses a method for preparing any of the above-mentioned textile auxiliary compositions, comprising:

[0024] (1) Add the mixed fatty acid glycerides into the reaction vessel and heat to melt;

[0025] (2) Weigh fatty acid alkoxylate, glyceryl monostearate and fatty alcohol alkoxylate into the reaction vessel in sequence, and stir and emulsify at a constant temperature;

[0026] (3) After emulsification, the product is obtained. Then, the product is transferred to the granulation and packaging line, weighed, packaged and stored.

[0027] Furthermore, the heating and melting temperature in step (1) is 70°C.

[0028] The present invention also discloses a textile auxiliary composition prepared according to the above preparation method.

[0029] The beneficial effects of this invention are as follows:

[0030] 1. The composition of this invention does not contain paraffin or non-environmentally friendly components. It uses low-value-added oil and fat chemical by-products as the main components, including hard cake PK1618, fatty acid recombinant components, and glycerol recombinant components. Among them, hard cake PK1618 is palm kernel oleic acid C1618, a by-product of obtaining oleic acid after freeze extraction. The fatty acid recombinant components are the residue after fatty acid distillation, and the glycerol recombinant components are the residue after glycerol distillation. These products have very low value, and even if they are disposed of by someone, improper disposal will affect the environment.

[0031] 2. This invention uses mixed fatty acid glycerides as the main raw material and adds a nonionic surfactant composition as an emulsifier to obtain a low-cost plant-based textile auxiliary composition. It can effectively solve the problem of by-products in the oleochemical industry, transforming low-value by-products into high-value-added products, and realizing waste recycling and sustainable production in the oleochemical industry. Detailed Implementation

[0032] The present invention will be further described below with reference to specific embodiments to aid in understanding its content. Unless otherwise specified, the methods used in this invention are conventional methods; the raw materials and apparatus used, unless otherwise specified, are conventional commercially available products.

[0033] Example 1

[0034] A textile auxiliary composition and its preparation method

[0035] (1) Preparation of mixed fatty acid glycerides: Add fatty acid byproducts (including: a mixture of palmitic acid, stearic acid and arachidic acid in any ratio) to a reaction vessel, heat to 90°C to melt, start stirring to obtain melted material, then add 4 parts of acidic catalyst by mass of fatty acids and introduce nitrogen gas; add glycerol byproducts dropwise at a fatty acid to glycerol mass ratio of 8:1, heat to 220°C and react for 6 hours until no obvious water is carried out, then stop the nitrogen gas introduction; then cool down to 165°C, start the water ring pump, and evacuate until no water is carried out, thus obtaining mixed fatty acid glycerides;

[0036] (2) Weigh 77 parts of mixed fatty acid glycerides and put them into the reaction vessel and heat them to 70°C to melt them; weigh 3 parts of fatty acid alkoxylate, 10 parts of glyceryl monostearate and 10 parts of fatty alcohol alkoxylate into the reaction vessel in sequence, and stir and emulsify them at a constant temperature.

[0037] (3) After emulsification, a textile auxiliary composition is obtained. Then, the product is transferred to the granulation and packaging line, weighed, packaged and stored.

[0038] Example 2

[0039] A textile auxiliary composition and its preparation method

[0040] (1) Preparation of mixed fatty acid glycerides: Add fatty acid byproducts (including: a mixture of palmitic acid, stearic acid and arachidic acid in any ratio) to a reaction vessel, heat to 90°C to melt, start stirring to obtain melted material, then add 4 parts of acidic catalyst by mass of fatty acids and introduce nitrogen gas; add glycerol byproducts dropwise at a fatty acid to glycerol mass ratio of 8:1, heat to 200°C and react for 7 hours until no obvious water is carried out, then stop the nitrogen gas introduction; then cool down to 160°C, start the water ring pump, and evacuate until no water is carried out, thus obtaining mixed fatty acid glycerides;

[0041] (2) Weigh 80 parts of mixed fatty acid glycerides and put them into the reaction vessel and heat them to 70°C to melt them; weigh 6 parts of fatty acid alkoxylate, 7 parts of glyceryl monostearate and 7 parts of fatty alcohol alkoxylate into the reaction vessel in sequence, and stir and emulsify them at a constant temperature.

[0042] (3) After emulsification, a textile auxiliary composition is obtained. Then, the product is transferred to the granulation and packaging line, weighed, packaged and stored.

[0043] Example 3

[0044] A textile auxiliary composition and its preparation method

[0045] (1) Preparation of mixed fatty acid glycerides: Add fatty acid byproducts (including: a mixture of palmitic acid, stearic acid and arachidic acid in any ratio) to a reaction vessel, heat to 90°C to melt, start stirring to obtain melted material, then add 4 parts of acidic catalyst by mass of fatty acids and introduce nitrogen gas; add glycerol byproducts dropwise at a fatty acid to glycerol mass ratio of 8:1, heat to 245°C and react for 5 hours until no obvious water is carried out, then stop the nitrogen gas introduction; then cool down to 170°C, start the water ring pump, and evacuate until no water is carried out, thus obtaining mixed fatty acid glycerides;

[0046] (2) Weigh 85 parts of mixed fatty acid glycerides and put them into the reaction vessel and heat them to 70°C to melt them; weigh 5 parts of fatty acid alkoxylate, 5 parts of glyceryl monostearate and 5 parts of fatty alcohol alkoxylate into the reaction vessel in sequence, and stir and emulsify them at a constant temperature.

[0047] (3) After emulsification, a textile auxiliary composition is obtained. Then, the product is transferred to the granulation and packaging line, weighed, packaged and stored.

[0048] Comparative Example 1

[0049] A textile wax sheet, the wax sheet being made from the following parts by weight: 70 parts of hydrogenated triglycerides, 18 parts of fatty acid esters, and 12 parts of fatty alcohol polyalkoxylates.

[0050] The hydrogenated triglycerides are selected from one or more combinations of palm oil, palm kernel oil, coconut oil, and soybean oil.

[0051] The fatty acid esters are selected from one or more combinations of Span20, Span40, Span60, Span80, etc.

[0052] The fatty alcohol polyalkoxylated compounds are selected from fatty alcohol polyoxyalkyl ethers.

[0053] Comparative Example 2

[0054] A textile wax sheet, the wax sheet being made from the following parts by weight: 90 parts hydrogenated triglycerides, 6 parts fatty acid esters, and 4 parts fatty alcohol polyalkoxylates.

[0055] The hydrogenated triglycerides are selected from one or more combinations of tallow, mutton tallow, and lard.

[0056] The fatty acid esters are selected from one or more combinations of monoglycerides, Tween20, Tween40, Tween60, Tween80, etc.

[0057] The fatty alcohol polyalkoxylates are selected from random, block, or alternating polymers of ethylene oxide and propylene oxide.

[0058] Test case

[0059] Performance testing

[0060] Emulsification performance test: Weigh 10g of the additive sample into a 200mL beaker, heat to 60-70℃ to melt, add 90g of deionized water, stir thoroughly, and observe whether the aqueous solution is a milky white homogeneous liquid. Cool to room temperature and observe whether the aqueous solution exhibits oil floating or clumping.

[0061] Smoothness test: Cotton fabric was used as the test object and cut into strips of 10cm*30cm. A 5g / L wax emulsion was prepared, and the cut cotton strips were soaked in the wax emulsion for 24 hours. After being taken out, they were dried with hot air at 100℃. After being fully rehydrated, they were sewn with a wireless electric sewing machine (46-50 stitches within 10cm). The number of broken yarns on the fabric surface within 10cm was counted (two unbroken yarns are counted as one broken yarn).

[0062] The performance test data results of Examples 1-3 and Comparative Examples 1-2 are as follows:

[0063] Table 1 Performance test results for each group

[0064] Emulsifying properties Stablize Stablize Stablize Layering clumping Smoothing performance 2 2 3 4 4

[0065] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A textile auxiliary composition, comprising: 60-90% by weight of mixed fatty acid glycerides; as well as The remainder is mixed with nonionic surfactants; wherein: The mixed fatty acid glycerides are a mixture of triglycerides, polyglycerides, mixed fatty acids, and polyglycerols obtained by esterification of oleochemical by-products. Mixed nonionic surfactants include: 2-10 parts fatty alcohol alkoxylates, 3-6 parts fatty acid alkoxylates, 3-10 parts glyceryl monostearate, wherein: The mixed fatty acid glycerides are prepared by the following method: (1) Add fatty acid byproducts to a reaction vessel and heat to melt them. Start stirring to obtain melted material. Then add acidic catalyst and purge with nitrogen. Fatty acid byproducts include a mixture of palmitic acid, stearic acid and arachidic acid. (2) Add glycerol byproduct dropwise at a fatty acid to glycerol mass ratio of 8:1, heat the reaction at 220-245℃ for 5-7 hours until no obvious water is carried out, then stop the nitrogen gas flow. (3) Cool down, start the water ring pump, and evacuate until no water is carried out.

2. The textile auxiliary composition according to claim 1, wherein: The heating temperature of the reactor in step (1) is 90°C.

3. The textile auxiliary composition according to claim 1, wherein: The reaction time in step (2) is 6 hours.

4. The textile auxiliary composition according to claim 1, wherein: Step (3) involves cooling the temperature to 160-170℃.

5. A method for preparing a textile auxiliary composition according to any one of claims 1 to 4, comprising: (1) Add the mixed fatty acid glycerides into the reaction vessel and heat to melt; (2) Weigh fatty acid alkoxylate, glyceryl monostearate and fatty alcohol alkoxylate into the reaction vessel in sequence, and stir and emulsify at a constant temperature; (3) After emulsification, the product is obtained. Then, the product is transferred to the granulation and packaging line, weighed, packaged and stored.

6. The preparation method according to claim 5, wherein: The melting temperature in step (1) is 70°C.

7. A textile auxiliary composition prepared by the method according to claim 5 or 6.

Citation Information

Patent Citations

  • Oiling agent used for natural fiber weaving, and preparation method thereof

    CN103911858A

  • Synthetic-fiber treatment agent and use thereof

    CN107849801A

  • Environment-friendly water-soluble textile wax and preparation method thereof

    CN107988797A

  • Method for deacidifying waste oil by glycerol method

    CN111454770A