CN116043538A - Softening agent in biological base bath and preparation method and application thereof - Google Patents
Softening agent in biological base bath and preparation method and application thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/46—Compounds containing quaternary nitrogen atoms
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/256—Sulfonated compounds esters thereof, e.g. sultones
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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Abstract
The invention belongs to the technical field of textile printing and dyeing in textile industry printing and dyeing production, and particularly relates to a softening agent in a biological base bath, a preparation method and application thereof. Firstly, adding bio-based organic fatty acid, a catalyst and organic amine in the reaction, mixing, carrying out dehydration reaction, adding a quaternizing reagent, carrying out quaternization reaction, and then compounding with a bio-based emulsifier and a defoaming agent to obtain a cationic softener; the natural oil sulfonated oil is added into the final product, so that the bio-based product can be completely biodegraded in the natural environment, the environment is protected, the safety is improved, and the renewable and environment-friendly value of the product is improved; the softening agent prepared by the invention utilizes the synergistic effect and the synergistic effect of the nonionic surfactant and the anionic surfactant, has good application effect, good fabric Huang Bianxiao, good hydrophilic performance and antistatic performance, meets the market demand, improves the product quality, and has remarkable social benefit and broad market prospect.
Description
Technical Field
The invention belongs to the technical field of textile printing and dyeing in textile industry printing and dyeing production, and particularly relates to a softening agent in a biological base bath, a preparation method and application thereof.
Background
With the continuous improvement of life quality, the wearing comfort of people is required to be higher and higher, the hand feeling of textiles after multiple processing and washing treatments in processing or daily use is rough, and the hand feeling of general synthetic fiber fabrics is poorer. In order to make the fabric soft, smooth and comfortable, the fabric needs to be finished, and the fabric is finished by using a softening agent widely used at present. The softening agent can enable the fiber to have soft smoothness which is suitable for processing conditions to avoid damage, so the softening agent is an important finishing agent which is necessary for improving the quality of products and increasing the added value of the products in textile printing and dyeing processing.
Cationic softeners are the most widely used types and include quaternary ammonium salts, silicone resins, esterquats, and the like. In addition, the organosilicon softener with good hand feeling has certain safety risk in use due to the fact that the raw materials contain siloxane ring bodies, and certain difficulty is caused in recovery in the use process of a printing and dyeing mill, so that the softener which does not contain silicon and has good hand feeling is needed in the market at present; meanwhile, the common silicon-free softener has poor biodegradability and serious yellowing, and with the improvement of public consciousness and environmental protection quality, the product can not meet the requirement of social development gradually.
Meanwhile, in recent years, with the enhancement of environmental awareness of people and the soundness of national environmental protection regulations, the reduction of petroleum reserves and the price rise and environmental pollution problems brought by petroleum-based polymer materials, the textile auxiliary needs to develop towards more green and environmental protection.
Disclosure of Invention
The invention aims to provide a biological-based softening agent in a bath, and a preparation method and application thereof.
To achieve the purpose, the invention adopts the following technical scheme:
a softening agent in a bio-based bath comprises raw materials of bio-based organic fatty acid, catalyst, organic amine, quaternizing agent, bio-based emulsifier, alcohol polymer, natural oil sulfonated oil, solvent and defoamer;
the total mass of the raw materials of the softener in the bath is calculated as 100%, and the mass percentage of each component is as follows:
the bio-based organic fatty acid is any one or any combination of saturated fatty acid of C12-C18, tall oil fatty acid and refined tall oil;
the catalyst is any one or any combination of hypophosphorous acid and p-toluenesulfonic acid.
The organic amine is any one or any combination of diethylenetriamine, triethanolamine and N, N-bis (3-aminopropyl) methylamine.
The quaternizing agent is any one or any combination of dimethyl carbonate, dimethyl sulfate, diethyl carbonate and diethyl sulfate.
The bio-based emulsifier is any one or any combination of anacardol polyoxyethylene ether NSS 1305 and A, NSS 1308 of the biotin-resistant organism.
The alcohol polymer is at least one or any combination of polyethylene glycol PEG400, PEG-600 and PEG-800.
The natural oil sulfonated oil is at least one or any combination of natural sulfonated rapeseed oil, natural sulfonated castor oil and sulfated natural beef tallow;
the solvent is at least one or any combination of diethylene glycol butyl ether, dipropylene glycol methyl ether and alcohol;
the defoamer is any one or any combination of polyoxypropylene polyoxyethylene glycerol ether and polyether modified polysiloxane.
A method for preparing a softener in a bio-based bath, comprising the steps of:
step one, mixing bio-based organic acid, a catalyst and organic amine, and starting dehydration reaction to obtain an initial product;
step two, adding a quaternizing reagent into the initial product obtained in the step one, and starting quaternization reaction;
step three, adding a bio-based emulsifier after the quaternization reaction in the step two is finished, so as to obtain the bio-based cationic softener;
and step four, after the bio-based cationic softener is uniformly mixed and stabilized in the step three, adding an alcohol polymer, natural oil sulfonated oil, a solvent and a defoaming agent to obtain the softener in the bio-based bath.
The preparation method of the softening agent in the bio-based bath comprises the following steps: under inert atmosphere, heating and melting the bio-based organic acid at 120-180 ℃ and stirring at 20-40rpm; adding a catalyst after melting, and uniformly stirring; then adding organic amine, heating to 180-230 ℃ to start dehydration reaction for 3-10 hours; the reaction was continued under vacuum for 0.5-3 hours to give the initial product.
The preparation method of the softening agent in the bio-based bath comprises the following steps: cooling to 70-90 ℃, slowly adding a quaternizing agent, controlling the charging time to be 1-3 hours, starting cooling water to control the reaction temperature, and continuing to keep the temperature for reaction for 1-3 hours after the addition is finished.
The preparation method of the softening agent in the bio-based bath comprises the following step: cooling to 70-80deg.C, adding bio-based emulsifier, and stirring.
The preparation method of the softening agent in the bio-based bath comprises the following steps: cooling to 50-60 ℃, adding alcohol polymer, natural oil sulfonated oil, solvent and defoamer, stirring uniformly, and filtering to obtain the softening agent in the bio-based bath.
In the invention, the natural oil sulfonated oil is added in an amount of 20-30%, and the stability of the softening agent in the bath is not obviously affected in the range.
The catalyst is 0.1% -1%, when the catalyst is lower than 0.1%, the reaction speed is slow, the heating and heat preserving time is prolonged, and the explosion is easy to occur; when the catalyst is more than 2%, the reaction speed is too high, the control is not easy, and the explosion polymerization is easy to generate during the reaction.
The defoamer is used in an amount of 0.01% -1%, for example 0.01%, 0.1%, 0.5% etc.
The defoaming agent is at least one of polyoxypropylene polyoxyethylene glycerol ether and polyether modified polysiloxane. Polyether modified polysiloxanes are preferred, so that the polyether modified polysiloxanes can quickly permeate into the foam in a high-temperature foaming system to damage the stability of the foam, thereby achieving the defoaming effect.
Preferably, the bio-based organic fatty acid is a saturated fatty acid of C12-C18;
preferably, the tall oil fatty acid is any one or any combination of ALTAPYNE 1483 from IngeCity, USA, HARTALL FA-1 from Japanese Ha Lima, and L1-C from Sonchuan technology (Fujian) Inc.
Preferably, the quaternizing agent is dimethyl sulfate.
Preferably, the natural oil sulfonated oil is at least one or any combination of natural sulfonated rapeseed oil, natural sulfonated castor oil and sulfated natural beef tallow;
preferably, the solvent is diethylene glycol butyl ether;
preferably, in the first step, the dehydration reaction temperature is 180-200 ℃ and the reaction time is 3-5 hours.
The biological base softening agent for bath is prepared by adopting the raw materials and the preparation method.
The application of the softener in the bio-based bath is characterized in that the softener in the bio-based bath or the softener in the bio-based bath prepared by any method is used for finishing textiles.
Advantageous effects
(1) The invention adopts the bio-based organic acid as the main body for reaction, thereby greatly reducing the consumption of fossil raw materials and improving the biodegradability and the added value of the product. Firstly, the adopted saturated fatty acid is stearic acid, namely C12-C18 saturated fatty acid, which is a fatty acid widely existing in nature, most enterprises producing stearic acid at home at present are imported palm oil from abroad, hydrogenation is carried out to obtain hardened oil, then hydrolysis distillation is carried out to obtain stearic acid, and the source is natural; secondly, the adopted tall oil fatty acid is derived from tall oil, and the processing and the utilization of the tall oil fatty acid are important components of circular economy, and relate to sustainable circular utilization of forest resources, have a larger linkage relation to ecological environment, and have larger economic benefit and social benefit. The modified low-carbon modified carbon fiber additive is prepared into a textile auxiliary raw material with proper performance, and the low-carbon and cyclic utilization of the textile raw material provides a powerful support for the green low-carbon sustainable development of the textile industry.
(2) The quaternization reaction is carried out in the preparation method, so that the hydrophilicity and permeability of the product are improved; the biological emulsifier is adopted, so that the hydrophilicity and permeability of the product are improved, and toxic and harmful substances are not generated at the same time, so that the sewage treatment pressure is not increased. When the softening agent in the biological base bath prepared by the invention is used for finishing textiles, the hand feeling, the softening performance, the color fastness performance and the anti-yellowing effect of the textiles can be effectively improved; meanwhile, a molecular channel can be formed on the textile, so that static electricity can be quickly transferred, and the antistatic performance of the textile is improved.
(3) The invention adds natural oil sulfonated oil, which is an anionic sulfonated oil fatliquor prepared by taking natural oil as a main raw material, adopting a sulfur trioxide gas sulfonation process to modify and compounding with other necessary components, is an excellent anionic surfactant, and can prevent fabric from causing rope wrinkles in bath or from being scratched to form color spots and hairiness; by utilizing the synergistic effect and synergy of the nonionic surfactant and the anionic surfactant, friction between fabrics and machines in the dyeing process is reduced, so that wrinkles, hairiness, scratches and chicken feet are prevented.
(4) The invention provides a biological-based softening agent in a bath and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing bio-based organic acid, a catalyst and organic amine, and starting dehydration reaction to obtain an initial product; adding a quaternizing agent to the polymer to initiate a quaternization reaction; and after the reaction is finished, adding a bio-based emulsifier, an alcohol polymer, natural oil sulfonated oil, a solvent and a defoaming agent to obtain the softening agent in the bio-based bath. The softening agent in the bath prepared by the invention has good application effect, and the fabric Huang Bianxiao has good hydrophilic performance and antistatic performance, thereby meeting the market demand; meanwhile, the raw materials and the production process adopted by the softener in the bio-based bath are environment-friendly, the product is safer to use, renewable and high in environment-friendly value.
(5) The bio-based product has good biodegradability, is environment-friendly, can reduce the use amount of traditional petroleum-based chemicals, has low production cost and obvious economic benefit, is produced cleanly, and is beneficial to protecting ecological environment. Along with the enhancement of people's environmental awareness and the soundness of national environmental regulations, the textile printing and dyeing industry needs to develop towards biomass, and the green sustainable development of the industry is realized.
Drawings
Fig. 1 is a flowchart of a preparation method of a softener in a bio-based bath according to an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples, in order to make the objects, technical solutions and advantages of the present invention more clear and clarified. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The raw materials for preparing the softener in the bio-based bath comprise bio-based organic fatty acid, catalyst, organic amine, quaternizing agent, bio-based emulsifier, alcohol polymer, natural oil sulfonated oil, solvent and defoamer;
the total mass of the raw materials of the softener in the bio-based bath is calculated as 100%, and the mass percentage of each component is as follows:
referring to fig. 1, fig. 1 is a flowchart of a preferred embodiment of a method for preparing a softening agent in a bio-based bath according to the present invention, as shown in the figure, comprising the steps of:
step one, mixing bio-based organic acid, a catalyst and organic amine, and starting dehydration reaction to obtain an initial product;
step two, adding a quaternizing reagent into the polymer to start quaternization reaction;
step three, adding a bio-based emulsifier after the reaction is finished;
and step four, adding an alcohol polymer, natural oil sulfonated oil, a solvent and a defoaming agent after uniformly mixing to obtain the softening agent in the bio-based bath.
In the embodiment, the long carbon chain ester amine with a hydrophilic chain segment structure is generated through the dehydration reaction of the bio-based organic acid and the organic amine, so that the softness of the softening agent in the prepared bio-based bath is ensured, and the hydrophilic performance and antistatic performance of the polymer are enhanced; finally, the polymer is mixed with a quaternizing agent to generate quaternization reaction to generate ester quaternary ammonium salt, so that the stability and anti-yellowing effect of the product are improved, and meanwhile, the hydrophilicity of the product is further improved.
In some embodiments, putting bio-based organic acid into a reaction kettle, heating and melting the mixture at the temperature of 75-85 ℃, introducing nitrogen after complete melting, adding a catalyst, heating to 140 ℃, then dropwise adding organic amine into the reaction kettle, heating to 186 ℃ after dropwise adding, performing dehydration reaction, performing constant temperature reaction for 3.5 hours, closing nitrogen, vacuumizing, and continuing constant temperature reaction for 0.5 hour to obtain an initial product; the initial product is a mixture of mono-and di-esters.
In the embodiment, under the action of a catalyst, the bio-based organic acid and the organic amine are mixed, so that the carboxyl of the bio-based organic acid and the amino or hydroxyl on the organic amine are subjected to dehydration reaction, the triester-free ester ammonium is synthesized, the adverse effect of the triester compound on the softness is avoided, and the generated long carbon chain structure can endow soft hand feeling to textiles. The embodiment adopts a nitrogen protection method, water generated by dehydration reaction can be taken away by introducing nitrogen, the reaction is facilitated, and meanwhile, due to the introduction of the nitrogen, raw materials are not oxidized by air at high temperature, so that the color of a product is ensured.
In some embodiments, the biobased organic acid is any one or any combination of a C12-C18 saturated fatty acid, tall oil fatty acid, refined tall oil.
In some embodiments, the catalyst is any one or any combination of hypophosphorous acid, para-toluene sulfonic acid.
In some embodiments, the organic amine is any one or any combination of diethylenetriamine, triethanolamine, and N, N-bis (3-aminopropyl) methylamine.
In some embodiments, the molar ratio of the biobased organic acid to the organic amine is (1-3) to 1. In the molar ratio range, the carboxyl group on the bio-based organic acid can be dehydrated with enough amino or hydroxyl groups on the organic amine, so that the synthetic product is ensured to be a mixture of monoester and diester, and the activity of the ester quaternary ammonium salt generated subsequently is stronger.
In some embodiments, the polymer is cooled to 75-80 ℃, quaternizing agent is added for quaternization reaction, the reaction is carried out for 1-3 hours, after the reaction is finished, the temperature is cooled to 70 ℃, bio-based emulsifier is added in proportion, alcohol polymer, natural oil sulfonated oil, solvent and defoamer are added in proportion, after the mixture is stirred uniformly, the mixture is filtered and discharged, and the softener in the bio-based bath is obtained.
In the embodiment, the quaternizing agent is added into the polymer, the hydrogen ions of the amino groups on the polymer are replaced, and the quaternary ammonium structure is free of hydrogen, so that a cationic surfactant is formed, and the hydrophilicity and the permeability of the textile can be further improved; the ester quaternary ammonium salt has good stability, good yellowing resistance and excellent biodegradability; emulsifying agent, alcohol polymer and solvent are added to improve the solubility and dispersibility of the product in water.
In some embodiments, the quaternizing agent is any one or any combination of dimethyl carbonate, dimethyl sulfate, diethyl carbonate, and diethyl sulfate.
In some embodiments, the bio-based emulsifier is any one or any combination of cardanol polyoxyethylene ether NSS 1305, NSS 1305A, NSS 1308 of a biotin-tolerant organism.
In some embodiments, the alcohol polymer is at least one of polyethylene glycol PEG400, PEG-600, PEG-800, or any combination thereof.
In some embodiments, the solvent is at least one of diethylene glycol butyl ether, dipropylene glycol methyl ether, alcohol, or any combination thereof.
In some embodiments, the natural oil sulfonated oil is added, and is an anionic sulfonated oil fatliquor prepared by modifying the natural oil sulfonated oil by a sulfur trioxide gas sulfonation process and then compounding the modified natural oil sulfonated oil with other necessary components, namely an excellent anionic surfactant. The hydrophilic chain segment can form a molecular channel on the fabric, so that static electricity on the surface of the fabric is quickly transferred, the antistatic effect of the fabric is realized, and the fabric can be prevented from causing rope wrinkles in a bath or from being scratched to form color spots and hairiness; during dyeing, the dynamic and static friction coefficients between fabrics and between the fabrics and the machine are reduced, thereby preventing wrinkles, hairiness, bruising and "chicken feet".
In some embodiments, the natural fatty sulfonated oil is at least one of natural sulfonated rapeseed oil, natural sulfonated castor oil, sulfated natural beef tallow, or any combination thereof.
In some embodiments, there is also provided the use of a softening agent in a bio-based bath in textile finishing. The softening agent in the bio-based bath prepared by the invention has environment-friendly source, and can effectively improve the softening performance, yellowing resistance and antistatic performance of fabrics when being used for textile finishing.
The present invention will be described in detail with reference to the following examples.
Example 1
250g of tall oil fatty acid, 150g of saturated fatty acid of C12-C18 are added into a reaction kettle, stirring and heating are started, the rotating speed is 20rpm, heating and melting are performed at the temperature of 140 ℃, nitrogen is introduced, and 1.0g of hypophosphorous acid 50% are added; heating to 140 ℃, adding 70.6g of diethylenetriamine, starting heating after the addition, adjusting the rotating speed to 40-50rpm, when the temperature reaches 186+/-3 ℃, keeping the temperature for 3.5 hours, guan Danqi, vacuumizing, and continuing to perform heat preservation reaction for 30 minutes; breaking vacuum, introducing nitrogen, cooling to 80-85 ℃, slowly adding 86.9g of dimethyl sulfate, starting a cooling coil, controlling the temperature to be not more than 90 ℃, controlling the adding time to be about 1 hour, and controlling the temperature to react for 80 minutes at 80 ℃ after the adding is finished; cooling to 70deg.C, adding 40g NSS 1305 and 50g NSS 1308, stirring for 30 min to emulsify uniformly; cooling to 55 ℃, adding 45g of PEG-600, 270g of natural sulfonated rapeseed oil, 45g of diethylene glycol butyl ether and 0.5g of defoamer, stirring for 30 minutes until emulsification is uniform, filtering while hot, and discharging to prepare the biological base softener in the bath.
Example 2
250g of tall oil fatty acid, 155g of stearic acid, stirring and heating are added into a reaction kettle, the rotating speed is 20rpm, the temperature is controlled to be 140 ℃, heating and melting are carried out, nitrogen is introduced, and 0.8g of hypophosphorous acid 50% is added; heating to 140 ℃, adding 104.1g of triethanolamine, starting heating after the addition, adjusting the rotating speed to 40-50rpm, reacting for 3.5 hours when the temperature reaches 190 ℃, guan Danqi, vacuumizing, and continuing to react for 30 minutes; breaking vacuum, introducing nitrogen, cooling to 70 ℃, slowly adding 87.0g of dimethyl sulfate, starting a cooling coil, controlling the temperature to be not more than 90 ℃, controlling the adding time to be about 1 hour, and controlling the temperature to be 70 ℃ after the adding is completed to react for 80 minutes; 40g NSS 1305 and 50g NSS 1308 are added and stirred for 30 minutes until the emulsification is uniform; cooling to 55 ℃, adding 45g of PEG-600, 300g of natural sulfonated rapeseed oil, 45g of diethylene glycol butyl ether and 0.5g of defoamer, stirring for 30 minutes until emulsification is uniform, filtering while hot, and discharging to prepare the biological base softener in the bath.
Example 3
250g of tall oil fatty acid, 155g of stearic acid, stirring and heating are added into a reaction kettle, the rotating speed is 20rpm, the temperature is controlled to be 140 ℃, heating and melting are carried out, nitrogen is introduced, and 0.8g of hypophosphorous acid 50% is added; heating to 140 ℃, adding 101.3g of N, N-bis (3-aminopropyl) methylamine, starting heating after the addition, adjusting the rotating speed to 40-50rpm, reacting for 3.5 hours when the temperature reaches 190 ℃, guan Danqi, vacuumizing, and continuing to react for 30 minutes while keeping the temperature; breaking vacuum, introducing nitrogen, cooling to 70 ℃, slowly adding 87.0g of dimethyl sulfate, starting a cooling coil, controlling the temperature to be not more than 90 ℃, controlling the adding time to be about 1 hour, and controlling the temperature to be 70 ℃ after the adding is completed to react for 80 minutes; 40g NSS 1305 and 50g NSS 1308 are added and stirred for 30 minutes until the emulsification is uniform; cooling to 55 ℃, adding 45g of PEG-600, 270g of natural sulfonated rapeseed oil, 45g of diethylene glycol butyl ether and 0.5g of defoamer, stirring for 30 minutes until emulsification is uniform, filtering while hot, and discharging to prepare the biological base softener in the bath.
Example 4
430g of tall oil fatty acid is added into a reaction kettle, stirring and heating are started, the rotating speed is 20rpm, heating and melting are carried out at the temperature of 140 ℃, nitrogen is introduced, and 1.0g of hypophosphorous acid 50% is added; heating to 140 ℃, adding 108.4g of triethanolamine, starting heating after the addition, adjusting the rotating speed to 40-50rpm, keeping the temperature for reaction for 3 hours when the temperature reaches 200+/-3 ℃, guan Danqi, vacuumizing, and continuing to perform heat preservation reaction for 30 minutes; breaking vacuum, introducing nitrogen, cooling to 75-80 ℃, slowly adding 52g of dimethyl sulfate, starting a cooling coil, controlling the temperature to be not more than 90 ℃, controlling the adding time to be about 1 hour, and controlling the temperature to be 80 ℃ for reaction for 60 minutes after the adding is finished; cooling to 70 ℃, adding 80g of NSS 1305 and 100g of NSS 1308, and stirring for 30 minutes until emulsification is uniform; cooling to 55 ℃, adding 45g of PEG-600, 300g of natural sulfonated rapeseed oil, 45g of diethylene glycol butyl ether and 0.6g of defoamer, stirring for 30 minutes until emulsification is uniform, filtering while hot, and discharging to prepare the biological base softener in the bath.
The softener is a textile auxiliary agent which can be adsorbed on the surface of textile fibers and smoothen the fibers so as to change the hand feeling and make the product more comfortable. Soft finishing is an important finishing step in textile printing and dyeing processing. In the processing process of textiles, the hand feeling of the textiles becomes rough after multiple treatments, and the synthetic fiber fabrics are generally worse, especially the superfine fiber fabrics, so that the textiles need to be finished in order to have soft, smooth and comfortable hand feeling, and the soft agent is widely used for finishing at present. The quality evaluation of the softener is carried out not only on the softening performance of the fabric, but also on the color light influence, the hydrophilic performance, the antistatic performance and the like of the fabric.
The present invention will be further described with reference to the following examples, which are provided only to aid in understanding the present invention and should not be construed as limiting the invention in any way.
Comparative example 1
Commercially available bath lotion contains HA-BH.
1. Physical Property testing
Physical properties of the softeners in the bio-based baths prepared by examples 1 to 4 of the present invention were tested and the results are shown in table 1:
TABLE 1
As can be seen from Table 1, the biological-based bath softener prepared by the method has the advantages of stable product, high content and good safety, is a softener which can be used for textile processing and daily washing, protecting and finishing of textiles, has high safety and has good application prospect.
2. Softener application performance test
The comparison test was performed between the softeners in the bio-based baths prepared in examples 1 to 4 above and the softener commonly used in the market, comparative example 1.
The examples and comparative examples were each diluted with hot water to an emulsion having a softener content of 15%, and tested for softness, yellowing, hydrophilic properties and antistatic properties:
1. soft performance evaluation method
The method comprises the following steps of adopting a padding process for all-cotton woven cloth to carry out treatment: preparing 20g/L working solution, padding once at 0.2MPa, shaping (150 ℃ multiplied by 90 s), and performing moisture regain evaluation.
Hand feel evaluation: the two cloth samples are evaluated by a hand touch method, the hand feeling of the original cloth is rated as 1 grade, and the best hand feeling rating is positioned as 5 grade. The evaluation and scoring are carried out by more than 3 test persons with odd numbers, and the average value is taken, so that the larger the numerical value is, the better the hand feeling is.
2. Whiteness and chromatic light evaluation method
Padding: preparing 20g/L working solution, padding once under 0.2MPa, shaping (150 ℃ multiplied by 90 s), constant temperature and humidity for 30 minutes, and testing by using a Datacolor color meter. The whiteness is compared with the untreated cloth sample, and the greater the whiteness change is, namely the greater the yellowing is.
3. Hydrophilic performance evaluation method
The method comprises the following steps of adopting a padding process for all-cotton woven cloth to carry out treatment: preparing 20g/L working solution, padding once at 0.2MPa, shaping (150 ℃ multiplied by 90 s), and keeping constant temperature and humidity for 30 minutes.
And (3) dripping water drops on the finished fabric, and measuring the time for the water drops to be fully spread on the fabric, wherein the shorter the time is, the better the hydrophilic performance is.
4. Antistatic performance evaluation method
Adopting polyester woven cloth, and treating by padding process: preparing 20g/L working solution, padding once at 0.2MPa, shaping (150 ℃ multiplied by 90 s), constant temperature and constant humidity for 30 minutes, and measuring the resistivity of the cloth cover by a surface resistance tester, wherein the smaller the resistivity is, the better the antistatic performance is.
The application performance test results are shown in table 2:
TABLE 2
As can be seen from Table 2, the fabric treated by the biomass softener prepared by the method has excellent hand feeling, good whiteness, difficult color change and good anti-yellowing effect. Meanwhile, the treated fabric also has excellent hydrophilicity and antistatic performance.
In summary, the invention provides a softener in a bio-based bath and a preparation method thereof, which comprises the steps of firstly, carrying out dehydration reaction on bio-based organic acid and organic amine to generate long-chain ester ammonium with a hydrophilic chain segment structure, so that the softness of the softener in the prepared bio-based bath is ensured, and the hydrophilic antistatic performance of a polymer is enhanced; finally, the polymer is mixed with a quaternizing agent to generate quaternization reaction to generate ester quaternary ammonium salt, so that the stability and anti-yellowing effect of the product are improved, and meanwhile, the hydrophilicity of the product is further improved. Finally, natural oil sulfonated oil is added, the natural oil is used as a main raw material, the natural oil is modified by a sulfur trioxide gas sulfonation process, and then the anionic sulfonated oil fatliquor is compounded with other necessary components, so that the anionic sulfonated oil fatliquor is an excellent anionic surfactant and has very strong hydrophilic performance, and a molecular channel can be formed on a fabric by a hydrophilic chain segment, so that static electricity on the surface of the fabric is quickly transferred, and the static friction coefficient and the dynamic friction coefficient between fabrics are reduced. By utilizing the synergistic effect and the synergistic effect of the nonionic surfactant and the anionic surfactant, the fabric can be prevented from causing rope wrinkles or from being scratched to form color spots and hairiness in the bath; the friction between fabrics and between the fabrics and the machine during dyeing is reduced, thereby preventing the phenomena of wrinkling, hairiness, abrasion and "chicken feet".
The preparation method of the invention can obtain the biological softening agent in the base bath with good hydrophilic performance, softness, static resistance and yellowing resistance, so as to improve the quality of textiles.
The applicant states that the present invention is illustrated by the above examples as well as the method of preparation and use of the bio-based bath according to the invention, but the invention is not limited to the above detailed methods, i.e. it is not meant that the invention must be carried out in dependence on the above detailed methods. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (10)
1. A bio-based bath softener characterized by:
the raw materials of the softener in the bath comprise bio-based organic fatty acid, catalyst, organic amine, quaternizing agent, bio-based emulsifier, alcohol polymer, natural oil sulfonated oil, solvent and defoamer;
the total mass of the raw materials of the softener in the bath is calculated as 100%, and the mass percentage of each component is as follows:
2. a bio-based bath softener according to claim 1, characterized in that:
the bio-based organic acid is any one or any combination of saturated fatty acid of C12-C18, tall oil fatty acid and refined tall oil;
the catalyst is any one or any combination of hypophosphorous acid and p-toluenesulfonic acid;
the organic amine is any one or any combination of diethylenetriamine, triethanolamine and N, N-bis (3-aminopropyl) methylamine;
the quaternizing agent is any one or any combination of dimethyl carbonate, dimethyl sulfate, diethyl carbonate and diethyl sulfate;
the bio-based emulsifier is any one or any combination of anacardol polyoxyethylene ether NSS 1305 and A, NSS 1308 of biotin-resistant organisms;
the alcohol polymer is at least one or any combination of polyethylene glycol PEG400, PEG-600 and PEG-800;
the natural oil sulfonated oil is at least one or any combination of natural sulfonated rapeseed oil, natural sulfonated castor oil and sulfated natural beef tallow;
the solvent is at least one or any combination of diethylene glycol butyl ether, dipropylene glycol methyl ether and alcohol;
the defoamer is any one or any combination of polyoxypropylene polyoxyethylene glycerol ether and polyether modified polysiloxane.
3. A method for preparing a softening agent in a bio-based bath, which is characterized by comprising the following steps:
step one, mixing bio-based organic acid, a catalyst and organic amine, and starting dehydration reaction to obtain an initial product;
step two, adding a quaternizing reagent into the initial product obtained in the step one, and starting quaternization reaction;
step three, adding a bio-based emulsifier after the quaternization reaction in the step two is finished, so as to obtain the bio-based cationic softener;
and step four, after the bio-based cationic softener is uniformly mixed and stabilized in the step three, adding an alcohol polymer, natural oil sulfonated oil, a solvent and a defoaming agent to obtain the softener in the bio-based bath.
4. A process for the preparation of a bio-based softening agent in a bath according to claim 3,
the first step comprises the following steps: under inert atmosphere, heating and melting the bio-based organic acid at 120-180 ℃ and stirring at 20-40rpm; adding a catalyst after melting, and uniformly stirring; then adding organic amine, heating to 180-230 ℃ to start dehydration reaction for 3-10 hours; the reaction was continued under vacuum for 0.5-3 hours to give the initial product.
5. A process for the preparation of a bio-based softening agent in a bath according to claim 3,
the second step comprises the following steps: cooling to 70-90 ℃, slowly adding a quaternizing agent, controlling the charging time to be 1-3 hours, starting cooling water to control the reaction temperature, and continuing to keep the temperature for reaction for 1-3 hours after the addition is finished.
6. A process for the preparation of a bio-based softening agent in a bath according to claim 3,
the third step comprises the following steps: cooling to 70-80deg.C, adding bio-based emulsifier, and stirring.
7. A process for the preparation of a bio-based softening agent in a bath according to claim 3,
the fourth step comprises the following steps: cooling to 50-60 ℃, adding alcohol polymer, natural oil sulfonated oil, solvent and defoamer, stirring uniformly, and filtering to obtain the softening agent in the bio-based bath.
8. A bio-based softener in a bath, prepared by the method of any one of claims 3-7.
9. Use of a softener in a bio-based bath, characterized in that the softener according to any one of claims 1-2 is used for the finishing of textiles.
10. Use of a softener in a biobased bath, characterized in that the softener in a biobased bath prepared by the method according to any one of claims 3-7 is used for finishing textiles.
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