CN111690072A - Preparation and application of polyaldehyde anti-crease finishing agent for cotton fabric - Google Patents
Preparation and application of polyaldehyde anti-crease finishing agent for cotton fabric Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a polyaldehyde acid crease-resistant finishing agent for cotton fabrics, and belongs to the field of non-ironing finishing. The invention takes oligosaccharide as a main raw material and prepares the carboxyl oligosaccharide aldehydic acid crease-resistant finishing agent by a two-step oxidation method. The finishing agent not only contains carboxyl, but also contains a large amount of aldehyde groups, can adopt a multi-carboxyl crease-resistant finishing theory, also can adopt an aldehyde crease-resistant finishing theory, realizes the combination of the two crease-resistant theories, and is a novel cotton fabric crease-resistant finishing agent. In the process of finishing cotton fabrics, a composite catalyst containing sodium hypophosphite and magnesium chloride, a nontoxic polyethylene softening agent and a JFC penetrating agent are added to prepare finishing liquid. The finishing agent is used for crease-resistant finishing of cotton fabrics, can improve the problems of strong crease-resistant finishing and large abrasion resistance loss in the past while ensuring excellent crease-resistant effect, and meanwhile, the fabrics have no yellowing phenomenon and have plump hand feeling.
Description
Technical Field
The invention relates to preparation and application of a polyaldehyde acid crease-resistant finishing agent for cotton fabrics, and belongs to the technical field of non-ironing finishing.
Background
Mature non-ironing crease-resistant finishing agents formed at present mainly comprise N-hydroxymethyl non-ironing finishing agents, polycarboxylic acid non-ironing finishing agents and acetal non-ironing finishing agents, and can endow fabrics with good crease resistance. N-methylol-type finishes, while providing excellent anti-wrinkle properties, release formaldehyde during finishing, storage and wear of the finished fabric, which can be a significant hazard to both the textile manufacturer and the user. Polybasic carboxylic acid finishing agents can also provide good crease resistance, but the price of the finishing agents is high, the finishing agents need to be finished and processed under a low acid condition, the strength loss of fabrics is high, the finished fabrics are easy to yellow, and the whiteness is poor. Although the acetal non-ironing finishing agent does not contain formaldehyde and has better washability and alkali hydrolysis resistance, the acetal non-ironing finishing agent has relatively lower reactivity and common crease-resistant effect, and meanwhile, the acetal non-ironing finishing agent has higher price and is often mixed with 2D resin for use. Therefore, a new formaldehyde-free crease-resistant finishing agent with higher safety, high reactivity and good crease-resistant effect needs to be developed.
Disclosure of Invention
In order to solve the problems, according to the invention, trehalose primary hydroxyl is selectively oxidized by a NaClO/NaBr/TEMPO system to prepare a carboxylated trehalose derivative, then sodium periodate is adopted to selectively oxidize and open a ring, so that the carboxylated trehalose obtains an aldehyde group reaction group, and finally the carboxylated trehalose uronic acid crease-resistant finishing agent is prepared through concentration, purification and freeze drying. In the process of finishing cotton fabrics, a composite catalyst containing sodium hypophosphite and magnesium chloride, a nontoxic polyethylene softening agent and a JFC penetrating agent are added to prepare finishing liquid. The finishing agent is used for crease-resistant finishing of cotton fabrics, can improve the problems of strong crease-resistant finishing and large abrasion resistance loss in the past while ensuring excellent crease-resistant effect, and meanwhile, the fabrics have no yellowing phenomenon and have plump hand feeling.
The first purpose of the invention is to provide a carboxyl oligosaccharide aldehydic acid, the polymerization degree of the oligosaccharide is 2-10 sugar, including trehalose, sucrose, maltose or lactose, and the general formula of the carboxyl oligosaccharide aldehydic acid is as follows:
wherein n is 0-9 and m is 1-10.
The second purpose of the invention is to provide a method for preparing carboxyl oligosaccharide aldehydic acid, which takes oligosaccharide as raw material, firstly adopts NaClO/NaBr/TEMPO system to oxidize primary hydroxyl in the oligosaccharide into carboxyl to obtain carboxyl oligosaccharide, and then adopts sodium periodate to carry out oxidative ring-opening on the carboxyl oligosaccharide to obtain carboxyl oligosaccharide aldehydic acid.
In one embodiment of the invention, the oligosaccharide is trehalose, sucrose, maltose or lactose.
In one embodiment of the invention, the method comprises the steps of:
(1) the preparation process of the carboxyl oligosaccharide comprises the following steps: mixing oligosaccharide, sodium bromide and TEMPO to prepare reaction solution, reacting at 0-10 deg.C and pH10-11 for 10-60min, adding ethanol to terminate reaction, adjusting pH to neutral, desalting, concentrating, centrifuging, filtering, and freeze drying to obtain carboxylated oligosaccharide powder; the molar ratio of the oligosaccharide to the sodium bromide to the TEMPO is 1 (2-8): (1-5);
(2) preparation process of carboxyl oligosaccharanic acid: preparing the carboxyl oligosaccharide prepared in the step (1) and periodate into a solution, and reacting for 1-5h at the temperature of 5-10 ℃ to obtain carboxyl oligosaccharide aldehyde acid; the molar ratio of the carboxyl oligosaccharide to the soluble periodate is 1:1-1: 4.
In one embodiment of the invention, the trehalose mass fraction of the reaction solution in the process (1) is 5 wt% to 10 wt%.
In one embodiment of the invention, the amount of sodium hypochlorite in process (1) is from 2 v/v% to 5 v/v%.
In one embodiment of the present invention, the reaction temperature in the process (1) is 0 to 10 ℃.
In one embodiment of the present invention, the molar ratio of carboxytrehalose to soluble periodate in process (2) is from 1:1 to 1: 4.
In one embodiment of the present invention, the mass fraction of carboxyl trehalose in the reaction solution in the process (2) is 5 wt% to 10 wt%.
In one embodiment of the present invention, the reaction temperature in the process (2) is 5 to 10 ℃.
In one embodiment of the present invention, the reaction time in the process (2) is 1 to 5 hours.
In one embodiment of the present invention, barium chloride is added after the reaction of the process (2) is finished to remove periodate and iodate impurities from the solution.
The third purpose of the invention is to provide the application of the carboxyl oligosuronic acid in anti-wrinkle.
The fourth purpose of the invention is to provide a crease-resistant finishing method for fabrics, which comprises the steps of putting the fabrics into the mixed solution of the carboxyl oligosaccharide aldehydic acid, the composite catalyst, the penetrating agent JFC and the polyethylene softener, soaking for two times and rolling for two times, controlling the liquid carrying rate of the fabrics to be 90-100%, pre-drying, baking, washing and drying.
In one embodiment of the present invention, the pH of the mixed solution is 4 to 6.
In one embodiment of the invention, the composite catalyst is sodium hypophosphite and magnesium chloride in a ratio of 1:1-1:5, and the dosage is 10-20 g/L.
In one embodiment of the invention, the pre-baking temperature is 80-100 ℃.
In one embodiment of the present invention, the pre-baking time is 2-5 min.
In one embodiment of the present invention, the baking temperature is 150-.
In one embodiment of the present invention, the baking time is 1-5 min.
A fifth object of the invention is to provide a fabric obtained by applying the finishing method.
The sixth purpose of the invention is to provide clothes and home textiles containing the fabric.
It is a seventh object of the present invention to provide an anti-wrinkle finishing agent containing the above carboxyl oligouronic acid.
In one embodiment of the invention, the anti-wrinkle finishing agent comprises, by mass volume percentage, 60-80g/L of the carboxyl oligosaccharide aldehydic acid, 10-20g/L of the composite catalyst, 10-20g/L of the penetrating agent JFC and 10-20g/L of the polyethylene softening agent; the composite catalyst is sodium hypophosphite and magnesium chloride, and the mass ratio of the sodium hypophosphite to the magnesium chloride is 1:1-1: 5.
The invention has the beneficial effects that:
(1) according to the invention, trehalose primary hydroxyl is selectively oxidized by a NaClO/NaBr/TEMPO system to prepare a carboxylated trehalose derivative, then sodium periodate is adopted to selectively oxidize and open the ring, so that the carboxylated trehalose obtains aldehyde group reaction groups, and the prepared anti-wrinkle finishing agent not only contains the carboxyl group reaction groups, but also contains a large number of aldehyde group reaction groups by utilizing the synergistic effect between two-step oxidation, has good crosslinking effect with cellulose, has excellent anti-wrinkle performance (the wrinkle recovery angle is more than or equal to 260 degrees), does not release formaldehyde (the formaldehyde release amount is 0), has small strength loss (the strength retention rate is 65-75 percent), and is not easy to yellow (the Hunter whiteness is more than or equal to 83.2).
(2) In the process of finishing cotton fabrics, a composite catalyst containing sodium hypophosphite and magnesium chloride, a nontoxic polyethylene softening agent and a JFC penetrating agent are added to prepare finishing liquid. The finishing agent is used for crease-resistant finishing of cotton fabrics, can improve the problems of strong crease-resistant finishing and large abrasion resistance loss in the past while ensuring excellent crease-resistant effect, and meanwhile, the fabrics have no yellowing phenomenon and have plump hand feeling. The carboxylated seaweed uronic acid crease-resistant finishing agent does not contain formaldehyde, is green and environment-friendly, ensures the safety of the finished fabric from the source, has simple and reliable preparation process and simple and convenient operation of the finishing process, and meets the requirements of green dyeing and finishing and ecological dyeing and finishing.
Drawings
FIG. 1 is a reaction equation of carboxyl trehalamic acid.
FIG. 2 is an infrared spectrum of trehalose, carboxytrehalose and carboxyglucuronic acid.
FIG. 3 shows trehalose13C nuclear magnetic spectrum.
FIG. 4 is a schematic representation of carboxytrehalose13C nuclear magnetic spectrum.
FIG. 5 is a schematic representation of carboxysaruronate13C nuclear magnetic spectrum.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
1. Test method for carboxyl content:
the total carboxyl content was determined by titration. Accurately weighing 0.25g carboxyl trehalose sample, completely dissolving with 50mL deionized water, adding 0.1066mol/L hydrochloric acid standard solution, stirring to mix thoroughly, and adjusting pH to 2.5. Titrating with 0.05mol/L sodium hydroxide standard solution, dropwise adding 0.50mL sodium hydroxide solution each time, fully reacting, and recording the pH value at the equilibrium. The volume of the sodium hydroxide solution consumed is used as an abscissa, the pH value is used as an ordinate, a curve with two break points is obtained, the volume of the sodium hydroxide solution corresponding to the first break point is V1(mL), the volume of the sodium hydroxide solution corresponding to the second break point is V2(mL), and the experiment is repeated three times to obtain an average value. The calculation formula for the total carboxyl group content A (mmol/g) is as follows:
in the formula (1), the reaction mixture is,
w is the mass of carboxyl trehalose, g;
c is the concentration of the sodium hydroxide standard solution, mol/L.
2. The method for testing the aldehyde group content comprises the following steps:
the total aldehyde content was determined by hydroxylamine hydrochloride-point titration. Weighing 0.100g carboxyl trehalamic acid sample, adding 25ml 0.25mol/l hydroxylamine hydrochloride solution, dripping 2 drops of 0.05% methyl orange solution, standing for 2h after fully dissolving, measuring the amount of HCl released by solution reaction by potentiometric titration with 0.1mol/l NaOH solution as titrant, and calculating the aldehyde group content according to the amount of consumed NaOH. The titration was stopped after the color of the solution changed from red to yellow (pH about 5) as the pH of the solution changed during the titration. The volume V of NaOH consumed was recorded.
The calculation formula for the total aldehyde group content B (mmol/g) is as follows:
V×0.001×nNaOH＝nCHOformula (2)
[CHO]＝nCHO/m0Formula (3)
In the formulas (2) and (3),
v is the consumption volume of sodium hydroxide, ml;
nNaOHthe molar concentration of NaOH is mol/l;
nCHOis the number of moles, mmol, of aldehyde groups in the sample;
m0is the mass of the sample, g.
3. Performance index that cotton fabric crease-resistant finishing should reach
The recovery angle of the folds is more than or equal to 270 degrees; the strength damage is less than or equal to 30 percent; the evenness of the cloth surface is more than or equal to 4 grade; the change rate of the washing size is +/-2 percent, and the water absorption is less than or equal to 15 seconds; the content of the formaldehyde on the cloth surface is less than or equal to 75 mg/kg.
Example 1: method for preparing carboxyl seaweed uronic acid
As shown in FIG. 1, the preparation process of carboxyl alginic acid is as follows:
(1) the preparation process of carboxyl trehalose comprises the following steps: trehalose, sodium bromide and TEMPO (tetramethylpiperidine nitroxide) are mixed according to a molar ratio of 1: 8: 0.01, preparing a reaction solution, dropwise adding 8.5ml of sodium hypochlorite (pH 10.5) solution at 5 ℃, keeping the pH 10.5 after completely dropwise adding, stirring for 30min, then adding ethanol (10ml) to terminate the reaction, adjusting the pH to be neutral, desalting and concentrating, centrifugally filtering, and freeze-drying to obtain carboxyl trehalose powder;
(2) preparation process of carboxyl alginic acid: preparing the carboxyl trehalose prepared in the step (1) and periodate into a solution according to the molar ratio of 1:4, reacting at 10 ℃ for 3 hours, adding 7.6g of barium chloride, reacting for 6 hours, centrifuging and filtering, and removing periodate and iodate in the solution to prepare the carboxyl trehalose uronic acid.
From the infrared spectrum (FIG. 2), 1629cm-1And 1417cm-1Is a characteristic absorption peak of carboxyl (-COONa) in the sample structure, 1628cm-1Characteristic absorption peaks of aldehyde groups (-C ═ OH) in the sample structure. From the nuclear magnetic spectra (FIGS. 3-5), characteristic chemical shifts of sodium carboxylates and aldehyde groups were found at 166.64ppm and 1663.22 ppm. The carboxyl seaweed uronic acid prepared by the method of the embodiment has a carboxyl content of 0.79mmol/g and an aldehyde content of 2.35 mmol/g. And the analysis of the content of carboxyl and aldehyde groups is combined to show that the carboxylated trehalose is successfully prepared.
Example 2: crease-resistant finishing of cotton fabric by using carboxyl seaweed uronic acid
It is known that the breaking strength of pure cotton plain cloth before finishing is 635.1N, the wrinkle recovery angle is 124.6 degrees, the Hunter whiteness is 93.2 cloth cover formaldehyde content is 0, the cloth cover flatness is 2.0 grade, and the washing size change rate is +/-5 percent.
The carboxyl seaweed uronic acid prepared in example 1 is used as a crease-resistant finishing agent for cotton fabrics, and the finishing process of the cotton fabrics is as follows: placing bleached cotton cloth in the carboxyl seaweed uronic acid finishing liquid prepared in the example 1, adding 10g/l of composite catalyst (hypophosphorous acid: magnesium chloride: 1:9), penetrating agent JFC and polyethylene softener in a mixed liquid, controlling the pH value to be 4, soaking twice and rolling twice, controlling the liquid carrying rate of the fabric to be 80-90%, the pre-drying temperature to be 80 ℃, the pre-drying time to be 3min, the baking temperature to be 150 ℃, the baking time to be 3min, washing with water and drying.
The crease recovery angle of the cotton fabric is 268.3 degrees, the strength retention rate is 82.1 percent, the Hunter whiteness is 83.2, the cloth cover formaldehyde content is 0, the cloth cover flatness is 3.4 grade and the washing size change rate is +/-2.5 percent according to national standards GB/T3923.1-2013, GB/T3819, GB/T17644-1998, GB/T2912.1-2009, FZ/T01147-2018 and GB/T8630-2013.
Example 3:
it is known that the breaking strength of pure cotton plain cloth before finishing is 635.1N, the wrinkle recovery angle is 124.6 degrees, the Hunter whiteness is 93.2 cloth cover formaldehyde content is 0, the cloth cover flatness is 2.0 grade, and the washing size change rate is +/-5 percent.
(1) The preparation process of carboxyl trehalose comprises the following steps: trehalose, sodium bromide and TEMPO (tetramethylpiperidine nitroxide) are mixed according to a molar ratio of 1: 8: 0.02 preparing a reaction solution, dropwise adding 8.5ml of sodium hypochlorite (pH 10.5) solution at 5 ℃, keeping the pH 10.5 after completely dropwise adding, stirring for 30min, then adding ethanol (10ml) to terminate the reaction, adjusting the pH to be neutral, desalting and concentrating, centrifugally filtering, and freeze-drying to obtain carboxyl trehalose powder;
(2) preparation process of carboxyl alginic acid: preparing the carboxyl trehalose prepared in the step (1) and periodate into a solution according to the molar ratio of 1:4, reacting at 10 ℃ for 3 hours, adding 7.6g of barium chloride, reacting for 6 hours, and performing centrifugal filtration to prepare the carboxyl trehalose uronic acid finishing agent.
(3) The cotton fabric finishing process comprises the following steps: putting bleached cotton cloth into the finishing liquid (2), adding a composite catalyst of 20g/l (hypophosphorous acid: magnesium chloride: 1:9), a penetrating agent JFC and a mixed liquid of a polyethylene softening agent, controlling the liquid carrying rate of the fabric to be 80-90%, controlling the pre-drying temperature to be 80 ℃, controlling the pre-drying time to be 3min, controlling the drying temperature to be 150 ℃, controlling the drying time to be 3min, washing and drying.
The carboxyl seaweed uronic acid non-ironing finishing agent prepared by the method has the carboxyl content of 0.92mmol/g and the aldehyde content of 2.40mmol/g, and the treated cotton fabric has the crease recovery angle of 270.6%, the strength retention rate of 79.3%, the Hunter whiteness of 80.2, the cloth cover formaldehyde content of 0, the cloth cover evenness of 3.1 grade and the water washing size change rate of +/-2% according to the national standards GB/T3923.1-2013, GB/T3819, GB/T17644-1998, GB/T2912.1-2009, FZ/T01147-2018 and GB/T8630-2013.
Example 4:
it is known that the breaking strength of pure cotton plain cloth before finishing is 635.1N, the wrinkle recovery angle is 124.6 degrees, the Hunter whiteness is 93.2 cloth cover formaldehyde content is 0, the cloth cover flatness is 2.0 grade, and the washing size change rate is +/-5 percent.
(1) The preparation process of carboxyl trehalose comprises the following steps: trehalose, sodium bromide and TEMPO (tetramethylpiperidine nitroxide) are mixed according to a molar ratio of 1: 8: 0.02 preparing a reaction solution, dropwise adding 8.5ml of sodium hypochlorite (pH 10.5) solution at 5 ℃, keeping the pH 10.5 after completely dropwise adding, stirring for 30min, then adding ethanol (10ml) to terminate the reaction, adjusting the pH to be neutral, desalting and concentrating, centrifugally filtering, and freeze-drying to obtain carboxyl trehalose powder;
(2) preparation process of carboxyl alginic acid: preparing the carboxyl trehalose prepared in the step (1) and periodate into a solution according to the molar ratio of 1:2, reacting at 10 ℃ for 3 hours, adding 7.6g of barium chloride, reacting for 6 hours, and performing centrifugal filtration to prepare the carboxyl trehalose uronic acid finishing agent.
(3) The cotton fabric finishing process comprises the following steps: putting bleached cotton cloth into the finishing liquid (2), adding a composite catalyst of 20g/l (hypophosphorous acid: magnesium chloride: 1:9), a penetrating agent JFC and a mixed liquid of a polyethylene softening agent, controlling the liquid carrying rate of the fabric to be 80-90%, controlling the pre-drying temperature to be 80 ℃, controlling the pre-drying time to be 3min, controlling the drying temperature to be 150 ℃, controlling the drying time to be 3min, washing and drying.
The carboxyl seaweed uronic acid non-ironing finishing agent prepared by the method has the carboxyl content of 0.92mmol/g and the aldehyde content of 1.80mmol/g, and the treated cotton fabric has the crease recovery angle of 256.3 degrees, the strength retention rate of 80.4 percent, the Hunter whiteness of 82.7, the cloth cover formaldehyde content of 0, the cloth cover evenness of 2.5 grade and the water washing size change rate of +/-3 percent according to the national standards GB/T3923.1-2013, GB/T3819, GB/T17644-1998, GB/T2912.1-2009, FZ/T01147-2018 and GB/T8630-2013.
Example 5:
it is known that the breaking strength of pure cotton plain cloth before finishing is 635.1N, the wrinkle recovery angle is 124.6 degrees, the Hunter whiteness is 93.2 cloth cover formaldehyde content is 0, the cloth cover flatness is 2.0 grade, and the washing size change rate is +/-5 percent.
(1) The preparation process of carboxyl trehalose comprises the following steps: trehalose, sodium bromide and TEMPO (tetramethylpiperidine nitroxide) are mixed according to a molar ratio of 1: 6: 0.02 preparing a reaction solution, dropwise adding 8.5ml of sodium hypochlorite (pH 10.5) solution at 5 ℃, keeping the pH 10.5 after completely dropwise adding, stirring for 30min, then adding ethanol (10ml) to terminate the reaction, adjusting the pH to be neutral, desalting and concentrating, centrifugally filtering, and freeze-drying to obtain carboxylated trehalose powder;
(2) preparation process of carboxyl alginic acid: preparing the carboxyl trehalose prepared in the step (1) and periodate into a solution according to the molar ratio of 1:3, reacting at 10 ℃ for 3 hours, adding 7.6g of barium chloride, reacting for 6 hours, and performing centrifugal filtration to prepare the carboxyl trehalose uronic acid finishing agent.
(3) The cotton fabric finishing process comprises the following steps: putting bleached cotton cloth into the finishing liquid (2), adding 10g/l of composite catalyst (hypophosphorous acid: magnesium chloride: 2:8), pH (potential of hydrogen) of a penetrating agent JFC and a mixed solution of polyethylene softener, soaking twice and rolling twice, controlling the liquid carrying rate of the fabric to be 80-90%, the pre-drying temperature to be 80 ℃, the pre-drying time to be 3min, the baking temperature to be 150 ℃, the baking time to be 3min, washing with water and drying.
The carboxyl seaweed uronic acid non-ironing finishing agent prepared by the method has the carboxyl content of 0.92mmol/g and the aldehyde content of 2.40mmol/g, and the treated cotton fabric has the crease recovery angle of 273.1%, the strength retention rate of 74.6%, the Hunter whiteness of 76.1, the cloth cover formaldehyde content of 0, the cloth cover evenness of 3.4 grade and the water washing size change rate of +/-3% measured according to the national standards GB/T3923.1-2013, GB/T3819, GB/T17644-1998, GB/T2912.1-2009, FZ/T01147-2018 and GB/T8630-2013.
Example 6:
it is known that the breaking strength of pure cotton plain cloth before finishing is 635.1N, the wrinkle recovery angle is 124.6 degrees, the Hunter whiteness is 93.2 cloth cover formaldehyde content is 0, the cloth cover flatness is 2.0 grade, and the washing size change rate is +/-5 percent.
(1) The preparation process of carboxyl trehalose comprises the following steps: trehalose, sodium bromide and TEMPO (tetramethylpiperidine nitroxide) are mixed according to a molar ratio of 1: 4: 0.02 preparing a reaction solution, dropwise adding 8.5ml of sodium hypochlorite (pH 10.5) solution at 5 ℃, keeping the pH 10.5 after completely dropwise adding, stirring for 30min, then adding ethanol (10ml) to terminate the reaction, adjusting the pH to be neutral, desalting and concentrating, centrifugally filtering, and freeze-drying to obtain carboxyl trehalose powder;
(2) preparation process of carboxyl alginic acid: preparing the carboxyl trehalose prepared in the step (1) and periodate into a solution according to the molar ratio of 1:4, reacting at 10 ℃ for 3 hours, adding 7.6g of barium chloride, reacting for 6 hours, and performing centrifugal filtration to prepare the carboxyl trehalose uronic acid finishing agent.
(3) The cotton fabric finishing process comprises the following steps: putting bleached cotton cloth into the finishing liquid (2), adding 15g/l of composite catalyst (hypophosphorous acid: magnesium chloride: 2:8), pH (potential of hydrogen) of a penetrating agent JFC and a mixed solution of polyethylene softener, soaking twice and rolling twice, controlling the liquid carrying rate of the fabric to be 80-90%, the pre-drying temperature to be 80 ℃, the pre-drying time to be 3min, the baking temperature to be 170 ℃, the baking time to be 2min, washing with water and drying.
The carboxyl seaweed uronic acid non-ironing finishing agent prepared by the method has the carboxyl content of 0.92mmol/g and the aldehyde content of 2.40mmol/g, and the treated cotton fabric has the crease recovery angle of 275.4 degrees, the strength retention rate of 71.6 percent, the Hunter whiteness of 70.1, the cloth cover formaldehyde content of 0, the cloth cover flatness of 2.8 grade and the water washing size change rate of +/-2.5 percent according to national standards GB/T3923.1-2013, GB/T3819, GB/T17644-1998, GB/T2912.1-2009, FZ/T01147-2018 and GB/T8630-2013.
Example 7:
it is known that the breaking strength of pure cotton plain cloth before finishing is 635.1N, the wrinkle recovery angle is 124.6 degrees, the Hunter whiteness is 93.2 cloth cover formaldehyde content is 0, the cloth cover flatness is 2.0 grade, and the washing size change rate is +/-5 percent.
(1) The preparation process of carboxyl sucrose comprises the following steps: mixing sucrose, sodium bromide and TEMPO (tetramethylpiperidine nitrogen oxide) according to a molar ratio of 1: 8: 0.02 preparing a reaction solution, dropwise adding 8.5ml of sodium hypochlorite (pH 10.5) solution at 5 ℃, maintaining the pH 10.5 after completely dropwise adding, stirring for 30min, then adding ethanol (10ml) to terminate the reaction, adjusting the pH to be neutral, desalting and concentrating, centrifugally filtering, and freeze-drying to obtain carboxyl sucrose powder;
(2) preparation process of carboxyl sucrose aldehydic acid: preparing the carboxyl sucrose and periodate prepared in the step (1) into a solution according to the molar ratio of 1:3, reacting at 10 ℃ for 3 hours, adding 7.6g of barium chloride, reacting for 6 hours, and performing centrifugal filtration to prepare the carboxyl sucrose aldehydic acid finishing agent.
(3) The cotton fabric finishing process comprises the following steps: putting bleached cotton cloth into the finishing liquid (2), adding a composite catalyst of 20g/l (hypophosphorous acid: magnesium chloride: 1:9), a penetrating agent JFC and a mixed liquid of a polyethylene softening agent, controlling the liquid carrying rate of the fabric to be 80-90%, controlling the pre-drying temperature to be 80 ℃, controlling the pre-drying time to be 3min, controlling the drying temperature to be 150 ℃, controlling the drying time to be 3min, washing and drying.
The carboxyl sucrose aldehydic acid non-ironing finishing agent prepared by the method has the carboxyl content of 1.32mmol/g and the aldehyde group content of 2.45 mmol/g. The crease recovery angle of the cotton fabric is 267.1 degrees, the strength retention rate is 80.5 percent, the Hunter whiteness is 76.4, the cloth cover formaldehyde content is 0, the cloth cover flatness is 3.1 grade and the washing size change rate is +/-3 percent according to national standards GB/T3923.1-2013, GB/T3819, GB/T17644-1998, GB/T2912.1-2009, FZ/T01147-2018 and GB/T8630-2013.
Example 8:
it is known that the breaking strength of pure cotton plain cloth before finishing is 635.1N, the wrinkle recovery angle is 124.6 degrees, the Hunter whiteness is 93.2 cloth cover formaldehyde content is 0, the cloth cover flatness is 2.0 grade, and the washing size change rate is +/-5 percent.
(1) The preparation process of carboxyl maltose: maltose, sodium bromide and TEMPO (tetramethylpiperidine nitroxide) are mixed according to a molar ratio of 1: 8: 0.02 preparing a reaction solution, dropwise adding 8.5ml of sodium hypochlorite (pH 10.5) solution at 5 ℃, maintaining the pH 10.5 after completely dropwise adding, stirring for 30min, then adding ethanol (10ml) to terminate the reaction, adjusting the pH to be neutral, desalting and concentrating, centrifugally filtering, and freeze-drying to obtain carboxyl maltose powder;
(2) preparation process of carboxymaltuluronic acid: preparing the carboxyl maltose prepared in the step (1) and periodate into a solution according to the molar ratio of 1:4, reacting at 10 ℃ for 3 hours, adding 7.6g of barium chloride, reacting for 6 hours, and performing centrifugal filtration to prepare the carboxyl maltouronic acid finishing agent.
(3) The cotton fabric finishing process comprises the following steps: putting bleached cotton cloth into the finishing liquid (2), adding a composite catalyst of 20g/l (hypophosphorous acid: magnesium chloride: 1:9), a penetrating agent JFC and a mixed liquid of a polyethylene softening agent, controlling the liquid carrying rate of the fabric to be 80-90%, controlling the pre-drying temperature to be 80 ℃, controlling the pre-drying time to be 3min, controlling the drying temperature to be 150 ℃, controlling the drying time to be 3min, washing and drying.
The carboxyl maltouronic acid non-ironing finishing agent prepared by the method has the carboxyl content of 0.82mmol/g and the aldehyde content of 1.84 mmol/g. The crease recovery angle of the cotton fabric is 245.8 degrees, the strength retention rate is 72.5 percent, the Hunter whiteness is 65.9, the cloth cover formaldehyde content is 0, the cloth cover flatness is 2.8 grade and the washing size change rate is +/-3.4 percent according to national standards GB/T3923.1-2013, GB/T3819, GB/T17644-1998, GB/T2912.1-2009, FZ/T01147-2018 and GB/T8630-2013.
Example 9:
it is known that the breaking strength of pure cotton plain cloth before finishing is 635.1N, the wrinkle recovery angle is 124.6 degrees, the Hunter whiteness is 93.2 cloth cover formaldehyde content is 0, the cloth cover flatness is 2.0 grade, and the washing size change rate is +/-5 percent.
(1) The preparation process of the carboxyl lactose comprises the following steps: lactose, sodium bromide and TEMPO (tetramethylpiperidine nitroxide) were mixed in a molar ratio of 1: 8: 0.03 preparing a reaction solution, dropwise adding 8.5ml of sodium hypochlorite (pH 10.5) solution at 5 ℃, maintaining the pH 10.5 after completely dropwise adding, stirring for 30min, then adding ethanol (10ml) to terminate the reaction, adjusting the pH to be neutral, desalting and concentrating, centrifugally filtering, and freeze-drying to obtain carboxyl lactose powder;
(2) preparation process of carboxyl lactobionic acid: preparing the carboxyl lactose prepared in the step (1) and periodate into a solution according to the mol ratio of 1:4, reacting at 10 ℃ for 3 hours, adding 7.6g of barium chloride, reacting for 6 hours, and performing centrifugal filtration to prepare the carboxyl lactobionic acid finishing agent.
(3) The cotton fabric finishing process comprises the following steps: putting bleached cotton cloth into the finishing liquid (2), adding a composite catalyst of 20g/l (hypophosphorous acid: magnesium chloride: 1:9), a penetrating agent JFC and a mixed liquid of a polyethylene softening agent, controlling the liquid carrying rate of the fabric to be 80-90%, controlling the pre-drying temperature to be 80 ℃, controlling the pre-drying time to be 3min, controlling the drying temperature to be 150 ℃, controlling the drying time to be 3min, washing and drying.
The carboxyl lactobionic acid non-ironing finishing agent prepared by the method has the carboxyl content of 0.56mmol/g and the aldehyde group content of 1.84 mmol/g. The crease recovery angle of the cotton fabric is 226.8 degrees, the strength retention rate is 75.2 percent, the Hunter whiteness is 75.6, the cloth cover formaldehyde content is 0, the cloth cover flatness is 3.0 grade and the water washing size change rate is +/-3.7 percent according to national standards GB/T3923.1-2013, GB/T3819, GB/T17644-1998, GB/T2912.1-2009, FZ/T01147-2018 and GB/T8630-2013.
Comparative example 1:
the cotton fabric was finished by referring to the methods of examples 1 and 2 except that the steps (1) and (2) were omitted and the cotton fabric was finished by using only trehalose as a finishing liquid under the same conditions as in examples 1 and 2, and the properties of the treated cotton fabric were shown in table 1.
Comparative example 2:
the cotton fabric was finished by referring to the methods of examples 1 and 2 except that the step (2) was omitted and trehalose was oxidized by using only the NaClO/NaBr/TEMPO system, and the other conditions were the same as those of examples 1 and 2, and the properties of the treated cotton fabric were shown in Table 1.
Comparative example 3:
the cotton fabric was finished by referring to the methods of examples 1 and 2 except that the step (1) was omitted and trehalose was oxidized by periodate alone under the same conditions as in examples 1 and 2, and the properties of the treated cotton fabric were as shown in table 1.
Comparative example 4:
the cotton fabric was finished by referring to the methods of examples 1 and 2 except that the order of steps (1) and (2) was interchanged, the other conditions were the same as those of examples 1 and 2, and the anti-wrinkle effect is shown in table 1.
TABLE 1
As can be seen from Table 1, the crease recovery angle of the cotton fabric (comparative example 2) after the trehalose is oxidized by independently adopting a NaClO/NaBr/TEMPO system is 182.3 degrees, which is 15.2 percent higher than the crease resistance of the comparative example 1; the wrinkle recovery angle of the cotton fabric (comparative example 3) after the trehalose is oxidized by adopting periodate alone is 223.3 degrees, which is improved by 41.2 percent compared with the wrinkle resistance of the comparative example 1; and the crease recovery angle of the cotton fabric (example 2) treated by trehalose through the NaClO/NaBr/TEMPO system and the periodate two-step oxidation is 268.3 degrees, the crease resistance is improved by 69.6 percent compared with that of comparative example 1, and the crease resistance is more superior to the sum (56.4 percent) of the effects of the single NaClO/NaBr/TEMPO system oxidation and the single periodate oxidation treatment, which shows that the NaClO/NaBr/TEMPO and periodate two-step oxidation mutually support the aspect of improving the crease resistance effect of the fabric and have a certain synergistic effect.
In conclusion, the invention prepares the multi-aldehyde acid crease-resistant finishing agent for cotton fabrics, the finishing agent has higher carboxyl content and aldehyde group content, and simultaneously provides a corresponding finishing method. The crease-resistant effect of the cotton fabric treated by the crease-resistant finishing agent is improved obviously, the crease recovery angle is improved by 130-150 degrees, the strength retention rate is high, the whiteness is not reduced obviously, and the crease-resistant finishing requirement of the cotton fabric can be met.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The carboxyl oligosaccharaide aldehydic acid is characterized in that the polymerization degree of the oligosaccharide is 2 to 10 sugar, and the oligosaccharide comprises trehalose, sucrose, maltose or lactose, and the carboxyl oligosaccharaide aldehydic acid has the general formula:
wherein n is 0-9 and m is 1-10.
2. The preparation method of carboxyl oligosaccharaide aldehyde acid of claim 1 is characterized in that oligosaccharide is used as raw material, primary hydroxyl in the oligosaccharide is oxidized into carboxyl by NaClO/NaBr/TEMPO mixed system to obtain carboxyl oligosaccharide, and then the carboxyl oligosaccharide is subjected to oxidative ring opening by sodium periodate to obtain carboxyl oligosaccharaide aldehyde acid; the oligosaccharide is trehalose, sucrose, maltose or lactose.
3. A method according to claim 2 or 3, characterized in that the method comprises the steps of:
(1) the preparation process of the carboxyl oligosaccharide comprises the following steps: mixing oligosaccharide, sodium bromide and TEMPO to prepare reaction solution, reacting at pH of 10-11 and temperature of 0-10 deg.C for 10-60min, adding ethanol to stop reaction, adjusting pH to neutral, desalting, concentrating, centrifuging, filtering, and freeze drying to obtain carboxylated oligosaccharide powder; the molar ratio of the oligosaccharide to the sodium bromide to the TEMPO is 1 (2-8): (1-5);
(2) preparation process of carboxyl oligosaccharanic acid: preparing the carboxyl oligosaccharide prepared in the step (1) and periodate into a solution, and reacting for 1-5h at the temperature of 5-10 ℃ to obtain carboxyl oligosaccharide aldehyde acid; the molar ratio of the carboxyl oligosaccharide to the soluble periodate is 1:1-1: 4.
4. An anti-wrinkle finish comprising the carboxy oligouronic acid according to claim 1.
5. Use of the carboxy oligouronic acid according to claim 1 for anti-wrinkle.
6. A fabric crease-resistant finishing method is characterized in that the method comprises the steps of putting the fabric into the carboxyl oligosaccharide aldehydic acid of claim 1, adding the composite catalyst, the penetrating agent JFC and the polyethylene softener, padding, baking, washing and drying.
7. The method according to claim 6, wherein the composite catalyst is sodium hypophosphite and magnesium chloride in a mass ratio of 1:1-1:5, and the total mass volume concentration of the composite catalyst is 10-20 g/L.
8. A fabric obtainable by the finishing process of claim 6 or 7.
9. A garment or home textile comprising the fabric of claim 8.
10. An anti-wrinkle finishing agent for cotton fabrics, which is characterized by comprising 60-80g/L of carboxyl oligosaccharide aldehydic acid as defined in claim 1, 10-20g/L of composite catalyst, 10-20g/L of penetrating agent JFC and 10-20g/L of polyethylene softener in percentage by mass and volume; the composite catalyst is sodium hypophosphite and magnesium chloride, and the mass ratio of the sodium hypophosphite to the magnesium chloride is 1:1-1: 5.
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