A method for preparing a dibasic sugar-based cross-linking agent and a method for preparing anti-wrinkle fabric using the dibasic sugar-based cross-linking agent

Abstract

The invention provides a method for preparing a diglycosyl crosslinking agent and a method for preparing anti-wrinkle fabrics using the diglycosyl crosslinking agent, and belongs to the technical field of fabric finishing. The invention adopts a diglycosyl crosslinking agent to mix with a weak polar organic solvent, and then reacts with a periodate aqueous solution under light-proof conditions, and freezes and treats the periodate under low temperature conditions to recover the periodate, so as to obtain a diglycosyl crosslinking agent mother liquor, and freeze-drying to obtain a diglycosyl crosslinking agent powder. The method improves the yield of the diglycosyl crosslinking agent and the recovery rate of the oxidant, and the preparation time of the crosslinking agent is short, thereby improving the preparation efficiency. The invention adopts a binary solvent system in which the solvent is a strong polar solvent water and a weak polar organic solvent, and the prepared diglycosyl crosslinking agent is not easy to form hemiacetal or acetal. The diglycosyl crosslinking agent prepared by the invention is used to treat the fabric, and a non-ironing fabric with high strength, low color difference, formaldehyde-free, and machine washable can be obtained.

Description

Technical Field

[0001] The invention relates to the technical field of fabric finishing, and in particular to a method for preparing a dibasic sugar-based crosslinking agent and a method for preparing anti-wrinkle fabrics by using the dibasic sugar-based crosslinking agent. Background Art

[0002] High-end clothing fabrics made from Xinjiang long-staple cotton and silk are comfortable, breathable, and anti-static. However, due to the large number of hydrogen bonds formed between the macromolecules of cotton fabrics and silk, cotton fabrics and silk clothing tend to wrinkle after machine washing.

[0003] Chemical cross-linking can improve the water resistance of cotton fabrics and silk macromolecules, reduce the plasticity of water molecules, and improve the wrinkle resistance of silk clothing, thereby improving the easy-care properties of cotton fabrics and silk clothing. Currently reported formaldehyde-free anti-wrinkle finishing agents are mainly polycarboxylic acids and polyaldehydes. Current literature reports the use of dibasic sugars (sucrose, cellobiose, maltose, trehalose) and tribasic sugars (raffinose) as raw materials to prepare cross-linking agents containing two aldehyde groups, four aldehyde groups, or six aldehyde groups. The oxidants are mainly periodate (NaIO4), heavy metals (Pb 4+ ) salt, 2,2,6,6-tetramethylpiperidinyl oxide (TEMPO), etc. Among them, periodate is the most reported to selectively oxidize ortho-dihydroxyl groups to aldehyde groups. The solvent used is mainly water, which has a lot to do with the fact that the above-mentioned dibasic sugars, tribasic sugars, and oxidants are all water-soluble substances. The main problems in preparing a polyaldehyde cross-linking agent using binary or ternary sugars as raw materials, periodate as an oxidant, and water as a solvent are as follows: 1. Formic acid is generated during the reaction, which catalyzes the hydrolysis of the ether bonds between sugar rings, thereby degrading them into monocyclic sugars, reducing the yield of the target product, and thus affecting the cross-linking effect of the polyaldehyde; 2. Iodate is generated during the reaction, and the recovery or removal of iodate in the solution is usually done by adding a barium salt (such as barium chloride) to form barium iodate, but this method cannot completely remove the oxidant. The oxidant rolled onto the fabric will have a certain destructive effect on the macromolecular structure of cotton fabrics and silk under the action of high temperature (100-150°C), thereby reducing the strength of the fabric; 3. The oxidized binary or ternary sugar cross-linking agent is very easy to form hemiacetal or acetal under the catalysis of formic acid, thereby reducing the cross-linking effect between the polyaldehyde cross-linking agent and the cotton fabric and silk.

[0004] Therefore, developing a formaldehyde-free anti-wrinkle finishing agent suitable for cotton fabrics and silk clothing fabrics is a problem to be solved at present. Summary of the invention

[0005] In view of this, the object of the present invention is to provide a method for preparing a diglycosyl cross-linking agent, comprising the following steps:

[0006] (1) dissolving a dibasic sugar in a weakly polar organic solvent, stirring and dissolving to obtain a dibasic sugar organic solution, dissolving a periodate in distilled water, stirring and dissolving in a light-proof condition to obtain a periodate aqueous solution;

[0007] (2) lowering the temperature of the disaccharide organic solution prepared in step (1) to room temperature, and dripping a light-shielded periodate aqueous solution into the disaccharide organic solvent to react under the condition of shielding from light and passing a protective gas;

[0008] (3) After the reaction is completed, the reaction solution is transferred to a -60°C to -20°C environment and frozen for 1 to 12 hours, and the excess periodate and the generated iodate are precipitated in the form of salt. The salt is recovered by vacuum filtration to obtain a mother solution of a diglycosyl cross-linking agent, which is then stored at -60°C to -20°C for future use;

[0009] (4) Drying the mother solution of the diglycosyl crosslinking agent under reduced pressure at -60 to -50°C and a pressure of 4 Pa ​​for 6 to 8 hours to obtain a water-free and organic solvent-free powder, namely the diglycosyl crosslinking agent.

[0010] The structure of the dibasic sugar-based cross-linking agent prepared by the present invention is as shown in formula (I):

[0011]

[0012] Preferably, the weakly polar organic solvent in step (1) is at least one of N,N-dimethylformamide, N,N-dimethylacetamide and dimethyl sulfoxide; the disaccharide is sucrose or maltose; and the concentration of the disaccharide in the disaccharide organic solution is 0.05-0.15 g / ml.

[0013] Preferably, the periodate in step (1) is at least one of sodium periodate and potassium periodate; and the concentration of periodate in the periodate aqueous solution is 0.2-0.3 g / ml.

[0014] Preferably, the molar ratio of the periodate to the dibasic sugar in step (1) is 3.2-4.5:1.

[0015] Preferably, the protective gas in step (2) is nitrogen or helium.

[0016] Preferably, the dropping speed in step (2) is 20 ml / min;

[0017] Preferably, the light-proof reaction temperature in step (2) is 5-15° C., and the light-proof reaction time is 30 minutes to 3 hours.

[0018] Another object of the present invention is to provide a process for processing wrinkle-resistant fabrics using the above-mentioned dibasic sugar-based crosslinking agent, comprising the following steps:

[0019] S1. Preparation of working solution: adding 0.5-5 g / L whiteness or color protection agent and catalyst to the mother solution of the diglycosyl crosslinking agent, and then adding an alkali agent to adjust the pH value of the mother solution to 2-5; adding a solvent to obtain a solution with an effective content of 5-8% of the diglycosyl crosslinking agent;

[0020] S2, application of crosslinking agent: immersing the fabric in the solution of step S1 by two dipping and two rolling methods, with the fabric carrying 90-110% of the solution, and then performing a crosslinking reaction;

[0021] S3. Impurity removal and washing: Place the baked fabric in a solution of 0.5-1 g / L soap flakes and 0.1-2 g / L sodium carbonate at a bath ratio of 5:1, and wash at 40-60°C for 5-10 minutes.

[0022] Preferably, the whiteness or color protection agent in step S1 is N-methylformamide or formamide;

[0023] The catalyst is formic acid, and the amount of the catalyst added is 0.1-1 g / L;

[0024] The alkali agent is sodium carbonate or sodium bicarbonate;

[0025] The solvent is water or a weak polar organic solvent; the weak polar organic solvent is any one or more of N,N-dimethylformamide, N,N-dimethylacetamide, and dimethyl sulfoxide.

[0026] Preferably, the cross-linking reaction process conditions in step S2 are: pre-baking at 110-130° C. for 10-30 seconds, and baking at 150-180° C. for 60 seconds to 300 seconds.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] The invention provides a method for preparing a diglycosyl crosslinking agent, wherein diglycosyl is mixed with a weak polar organic solvent, and then reacted with a periodate aqueous solution under light-proof conditions, and then subjected to freezing treatment under low temperature conditions to recover excess periodate and generated iodate to obtain a diglycosyl crosslinking agent mother liquor, and freeze-dried to obtain a diglycosyl crosslinking agent powder. The method of the invention improves the yield of the diglycosyl crosslinking agent, the yield exceeds 99%, and the recovery rate of the oxidant is close to 100%; the preparation time of the crosslinking agent of the invention is short, and the preparation efficiency is improved. The invention adopts a binary solvent system in which the solvent is a strong polar solvent water and a weak polar organic solvent, and the prepared diglycosyl crosslinking agent is not easy to form hemiacetal or acetal. The diglycosyl crosslinking agent prepared by the invention is used to treat fabrics, and a non-ironing fabric with high strength, low color difference, no formaldehyde, and machine washable can be obtained; the organic solvent can also play the role of a penetrant and anti-yellowing function in the crosslinking reaction. The anti-wrinkle fabric processed by the present invention has an appearance grade of greater than or equal to 4.0 before washing, an appearance grade of greater than or equal to 3.5 after washing 50 times, a tear strength retention rate of more than 90%, a wrinkle recovery angle of more than 300 degrees, a whiteness retention rate of more than 90% for white fabrics, and a dry rubbing color fastness of dyed fabrics of greater than or equal to 4.0 and a wet rubbing color fastness of greater than or equal to 3.0. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 The ATR spectrum of the diglycosyl cross-linking agent prepared in Example 1;

[0030] Figure 2 The carbon NMR spectrum of the diglycosyl cross-linking agent prepared in Example 1;

[0031] Figure 3 The ATR spectrum of the sucrose aldehyde finishing agent prepared in Comparative Example 1;

[0032] Figure 4 This is the carbon nuclear magnetic resonance spectrum of the sucrose aldehyde finishing agent prepared in Comparative Example 1;

[0033] Figure 5 This is the carbon nuclear magnetic resonance spectrum of the sucrose aldehyde finishing agent prepared in Comparative Example 2. DETAILED DESCRIPTION

[0034] The present invention will be further described below in conjunction with the embodiments.

[0035] Example 1

[0036] A method for preparing a dibasic sugar-based cross-linking agent, comprising the following steps:

[0037] (1) 50 g (0.146 mol) of sucrose was added to 500 ml of N,N-dimethylformamide, and the mixture was dissolved by magnetic stirring at a speed of 800 rpm for about 10 minutes; 125 g (0.58 mol) of sodium periodate was added to 500 ml of distilled water to obtain a sucrose organic solution, and the sodium periodate aqueous solution was protected from light, and the mixture was dissolved by magnetic stirring at a speed of 800 rpm for about 15 minutes to obtain a sodium periodate aqueous solution;

[0038] (2) lowering the temperature of the sucrose organic solution prepared in step (1) to room temperature, introducing high-purity nitrogen as a protective gas, protecting the sucrose organic solvent solution from light, and then adding the light-protected sodium periodate solution dropwise using a constant pressure separatory funnel at a rate of 20 ml / min. After the addition is completed, reacting at 10° C. for 2 hours;

[0039] (3) After the reaction, the reaction solution was transferred to a -30°C environment and frozen for 5 hours. Excess sodium periodate and generated sodium iodate precipitated in the form of salt. The salt was recovered by low-temperature -30°C vacuum filtration. The residual oxidant was tested with starch potassium iodide test paper, and it was found that the test paper did not turn blue. The recovery rate of the oxidant was found to be 99.8% through titration analysis, indicating that the oxidant was well recovered. The obtained binary sugar-based cross-linking agent mother solution was stored in a -20°C environment for future use;

[0040] (4) The mother solution of the diglycosyl crosslinking agent was dried under reduced pressure at -60°C and 4 Pa ​​for 6 hours to obtain a water-free and organic solvent-free powder, namely the diglycosyl crosslinking agent. The aldehyde content of the diglycosyl crosslinking agent was 12.89 mmol / g, and the yield of the target product was calculated to be 99.2%.

[0041] The diglycosyl crosslinking agent powder prepared in Example 1 was taken and the types of newly generated chemical groups on its molecular structure were characterized by attenuated total reflection (ATR) technology. The ATR spectrum is as follows: Figure 1 ; The structure of the above oxidants is tracked by carbon nuclear magnetic resonance spectroscopy (C NMR) technology. Figure 2 .

[0042] from Figure 1 It can be found in the ATR spectrum that it appears at 1717 -1 The new peak of cm is the peak of aldehyde group. Figure 2 It can be found in the carbon NMR spectrum that there are two aldehyde peaks at 164 and 166 ppm respectively, which is basically consistent with the result of fitting two aldehyde peaks by ChemDraw 20.0 software.

[0043] Existing literature reports that the NMR carbon spectrum of the sucrose tetraaldehyde crosslinker has only one aldehyde peak, while the characterization results of the present invention show that the NMR carbon spectrum of the sucrose tetraaldehyde crosslinker has two aldehyde peaks. The reasons are as follows:

[0044] 1. The traditional preparation methods of sucrose tetraaldehyde crosslinking agents are all in aqueous solution. In theory, the hydrogen ions ionized by the oxidation byproduct formic acid can easily catalyze the reaction of the aldehyde group and hydroxyl group in the sucrose ring molecule to form hemiacetal, as reported in the paper (Oxysucrose polyaldehyde: A new hydrophilic crosslinking reagent for anti-crease finishing of cotton fabrics. Carbohydrate Research 2019, 486, 107783.);

[0045] 2. The generated oxidized sucrose will form intermolecular hemiacetal under the catalysis of hydrogen ions ionized from the oxidation by-product formic acid, which slows down the selective oxidation rate of the ortho-hydroxyl groups in the sucrose molecules by sodium periodate, and also reduces the yield of the sucrose-based tetraaldehyde cross-linker, so the two aldehyde groups cannot be detected.

[0046] In the present invention, sucrose is pre-dissolved in a non-protonic solvent N,N-dimethylformamide, and sodium periodate is dissolved in distilled water. After the two solutions are mixed, the amide group in the molecular structure of N,N-dimethylformamide can form a hydrogen bond with the hydrogen atom in the water molecule. The by-product formic acid cannot be ionized, so it will not catalyze the sucrose-based tetraaldehyde cross-linking agent to generate intramolecular and intermolecular hemiacetals.

[0047] Example 2

[0048] A method for processing a non-ironing white silk fabric, comprising the following steps:

[0049] S1. Preparation of working solution: 500 ml of the mother solution of the diglycosyl crosslinking agent was prepared according to the method of Example 1, and 0.5 g / L of N-methylformamide was added as a white protective agent; 0.5 g / L of formic acid was added as a catalyst, and 0.3 g / L of sodium carbonate was added to adjust the pH value of the working solution to 3.9; a weakly polar organic solvent N,N-dimethylformamide was added to make the effective content of the diglycosyl crosslinking agent 5%;

[0050] S2, application of crosslinking agent: immerse the white silk fabric in the solution of step S1 by two dipping and two rolling, the fabric carrying liquid volume is 100%, and then carry out crosslinking reaction; crosslinking reaction process conditions: pre-baking at 110° C. for 20 seconds, baking at 150° C. for 180 seconds;

[0051] S3. Impurity removal and washing: the baked fabric is placed in a solution of 0.5 g / L soap flakes and 0.1 g / L sodium carbonate at a bath ratio of 5:1, and washed at 50°C for 5 minutes.

[0052] The processed silk fabric has an appearance grade greater than or equal to 4.0 before washing according to GB / T 18863-2002, and an appearance grade greater than or equal to 3.5 after washing 50 times. The formaldehyde content measured according to GB / T 18401 is 0, the tear strength retention rate measured according to GB / T 3923.1 is 92.3%, the wrinkle recovery angle (warp + weft) of the fabric measured according to GB / T 319-1997 is 312 degrees, and the whiteness of the fabric is tested according to GB / T 8424.2-2001, and the whiteness retention rate is 95.2%.

[0053] Example 3

[0054] A method for processing a non-ironing dyed silk fabric, comprising the following steps:

[0055] S1. Preparation of working solution: 500 ml of the mother solution of the diglycosyl crosslinking agent was prepared according to the method of Example 1, and 1 g / L of N-methylformamide was added as a color protection agent; 0.6 g / L of formic acid was added as a catalyst, and 0.2 g / L of sodium carbonate was added to adjust the pH value of the working solution to 3.2; a weakly polar organic solvent N,N-dimethylformamide was added to make the effective content of the diglycosyl crosslinking agent 5%;

[0056] S2, application of crosslinking agent: immerse the dyed silk fabric in the solution of step S1 by two dipping and two rolling, the fabric carrying liquid volume is 100%, and then carry out crosslinking reaction; crosslinking reaction process conditions: pre-baking at 110° C. for 15 seconds, baking at 150° C. for 180 seconds;

[0057] S3. Impurity removal and washing: the baked fabric is placed in a solution of 0.5 g / L soap flakes and 0.1 g / L sodium carbonate at a bath ratio of 5:1, and washed at 50°C for 5 minutes.

[0058] The aldehyde content of the dibasic sugar-based cross-linking agent prepared by the method is 12.89 mmol / g. The appearance grade of the processed silk fabric measured according to GB / T 18863-2002 is greater than or equal to 3.9 before washing, and the appearance grade after 50 washings is greater than or equal to 3.5. The formaldehyde content measured according to GB / T 18401 is 0, the tear strength retention rate measured according to GB / T 3923.1 is 93.5%, the wrinkle recovery angle (warp + weft) of the fabric measured according to GB / T 319-1997 is 308 degrees, the dry friction color fastness of the fabric measured according to GB / T 3920-2008 is ≥4.0, and the wet friction color fastness is ≥3.0, the light fastness of the fabric measured according to GB / T 8427-2019 is ≥3.0, and the light fastness of the fabric measured according to GB / T 3921.1-2008 The washing color fastness of the tested fabric is basically ≥4.0.

[0059] Example 4

[0060] A method for processing non-ironing white cotton fabric, comprising the following steps:

[0061] S1. Preparation of working solution: 500 ml of the mother solution of the diglycosyl crosslinking agent was prepared according to the method of Example 1, and 1 g / L of N-methylformamide was added as a whiteness protection agent; 0.7 g / L of formic acid was added as a catalyst, and 0.01 g / L of sodium carbonate was added to adjust the pH value of the working solution to 2.3; a weakly polar organic solvent N,N-dimethylformamide was added to make the effective content of the diglycosyl crosslinking agent 5%;

[0062] S2, application of crosslinking agent: immerse the white cotton fabric in the solution of step S1 by two dipping and two rolling, the fabric carrying liquid volume is 100%, and then carry out crosslinking reaction; crosslinking reaction process conditions: pre-baking at 120°C for 15S, baking at 150°C for 240S;

[0063] S3. Impurity removal and washing: the baked fabric is placed in a solution of 0.5 g / L soap flakes and 0.1 g / L sodium carbonate at a bath ratio of 5:1, and washed at 50°C for 5 minutes.

[0064] The aldehyde content of the dibasic sugar-based cross-linking agent prepared by the method is 12.89 mmol / g. The appearance grade of the processed white cotton fabric measured according to GB / T 18863-2002 is greater than or equal to 4.0 before washing, and the appearance grade after 50 washings is greater than or equal to 3.5. The formaldehyde content measured according to GB / T 18401 is 0, the tear strength retention rate measured according to GB / T 3923.1 is 94.6%, the wrinkle recovery angle (warp + weft) of the fabric measured according to GB / T 319-1997 is 302 degrees, and the whiteness of the fabric is tested according to GB / T 8424.2-2001, and the whiteness retention rate is 92.2%.

[0065] Example 5

[0066] A method for processing a non-ironing dyed cotton fabric, comprising the following steps:

[0067] S1. Preparation of working solution: 500 ml of the mother solution of the diglycosyl crosslinking agent was prepared according to the method of Example 1, and 1 g / L of N-methylformamide was added as a whiteness protection agent; 0.75 g / L of formic acid was added as a catalyst, and 0.01 g / L of sodium carbonate was added to adjust the pH value of the working solution to 2.2; a weakly polar organic solvent N,N-dimethylformamide was added to make the effective content of the diglycosyl crosslinking agent 5%;

[0068] S2, application of crosslinking agent: immerse the dyed cotton fabric in the solution of step S1 by two dipping and two rolling, the fabric carrying liquid volume is 100%, and then carry out crosslinking reaction; crosslinking reaction process conditions: pre-baking at 110°C for 15S, baking at 150°C for 180S;

[0069] S3. Impurity removal and washing: the baked fabric is placed in a solution of 0.5 g / L soap flakes and 0.1 g / L sodium carbonate at a bath ratio of 5:1, and washed at 50°C for 5 minutes.

[0070] The aldehyde content of the dibasic sugar-based cross-linking agent prepared by the method is 12.89 mmol / g. The appearance grade of the processed silk fabric measured according to GB / T 18863-2002 is greater than or equal to 3.8 before washing, and the appearance grade after 50 washings is greater than or equal to 3.5. The formaldehyde content measured according to GB / T 18401 is 0, the tear strength retention rate measured according to GB / T 3923.1 is 93.5%, the wrinkle recovery angle (warp + weft) of the fabric measured according to GB / T 319-1997 is 301 degrees, the dry friction color fastness of the fabric measured according to GB / T 3920-2008 is ≥4.0, and the wet friction color fastness is ≥3.0, the light fastness of the fabric measured according to GB / T 8427-2019 is ≥3.0, and the light fastness of the fabric measured according to GB / T 3921.1-2008 The washing color fastness of the tested fabric is basically ≥4.0.

[0071] Comparative Example 1

[0072] A method for preparing a sucrose aldehyde finishing solution, comprising the following steps:

[0073] According to the method of invention patent CN 108998970 B, a certain amount of sucrose is added to distilled water, wherein the mass fraction of sucrose is 5%, the molar ratio of sodium periodate to sucrose is 3:1, the reaction solution is reacted at 20°C for 26 hours, and then barium chloride is added at a molar ratio of 1:2 to sodium periodate. After stirring for 1 hour, the mixture is filtered to obtain a clear liquid as the sucrose aldehyde cross-linking agent.

[0074] The titration test showed that the aldehyde content was 6.7 mmol / g, which indicated that part of the sucrose was not oxidized or the oxidized sucrose formed intramolecular hemiacetal, resulting in a lower aldehyde content. The titration test showed that the residual rate of sodium iodate was 13.2%. 10 ml of the above liquid was taken and dried under reduced pressure at -60°C and 4 Pa ​​pressure for 3 hours to obtain an anhydrous powdered sucrose aldehyde finishing agent.

[0075] Take the above powder and characterize the types of newly generated chemical groups in its molecular structure by attenuated total reflection (ATR) technology. The results are as follows: Figure 3 ; The structure of the above oxidants is tracked by carbon nuclear magnetic resonance spectroscopy (C NMR) technology. Figure 4 .

[0076] from Figure 3 It can be found in the ATR spectrum that it appears at 1722 -1 The new peak of cm is the peak of aldehyde group. Figure 4 It can be found in the carbon nuclear magnetic resonance spectrum that there is only one aldehyde peak at 164ppm. This is mainly because sucrose aldehyde forms an intramolecular hemiacetal in aqueous solution under the catalysis of formic acid.

[0077] Comparative Example 2

[0078] A method for preparing a sucrose aldehyde finishing solution, comprising the following steps:

[0079] The reaction solution was reacted at 20°C for 3 hours, and the remaining steps and conditions were the same as those in Comparative Example 1. Figure 5 , Figure 5 No aldehyde peak was observed, indicating that the oxidation reaction takes a long time in a water system.

[0080] Comparative Example 3

[0081] A method for processing wrinkle-resistant cotton fabric, comprising the following steps:

[0082] According to the method of invention patent CN 108998970 B, 20 g / L of magnesium chloride, 2 g / L of penetrant (JFC, composed of fatty alcohol polyoxyethylene ether) and 2 g / L of softener (NP-825, composed of polyethylene emulsion) were added to the finishing solution of comparative example 1, and the pH value was 3. The bleached cotton fabric was dipped and padded in the finishing solution, dipped and padded twice, and the liquid carrying rate of the fabric was controlled to be 90%, the pre-baking temperature was 80°C, the time was 10 minutes, the baking temperature was 120°C, the baking time was 1 minute, and the fabric was washed and dried.

[0083] The strength retention rate of cotton fabric is 86.3%, the wrinkle recovery angle is 205 degrees, and the whiteness retention rate is 92.1%. The hemiacetal formed by sucrose aldehyde in the molecule will reduce the number of reactive groups on the cross-linking agent, thereby reducing the anti-wrinkle effect.

[0084] Comparative Example 4

[0085] A method for processing wrinkle-resistant silk fabric, comprising the following steps:

[0086] 20 g / L of magnesium chloride, 2 g / L of penetrant (JFC, fatty alcohol polyoxyethylene ether) and 2 g / L of softener (NP-825, polyethylene emulsion) were added to the finishing solution of Comparative Example 1, pH = 3. The bleached cotton fabric was dipped and padded in the finishing solution, double dip and double padded, the fabric liquid carrying rate was controlled to be 90%, the pre-baking temperature was 80°C, the time was 10 minutes, the baking temperature was 150°C, the baking time was 5 minutes, and the fabric was washed and dried.

[0087] The strength retention rate of silk fabric is 76.3%, the wrinkle recovery angle is 235 degrees, and the whiteness retention rate is 82.1%. The hemiacetal formed by sucrose aldehyde in the molecule will reduce the number of reactive groups on the crosslinking agent, thereby reducing the anti-wrinkle effect. As reported in the paper (Oxysucrose polyaldehyde: A new hydrophilic crosslinking reagent for anti-crease finishing of cotton fabrics. Carbohydrate Research 2019, 486, 107783.).

[0088] Comparative Example 5

[0089] Take 50 grams of sucrose and 31.25 grams of sodium periodate, and the remaining steps and conditions are the same as those in Example 1. The dibasic sugar-based cross-linking agent prepared by this method has an aldehyde content of 5.75 mmol / g.

[0090] Comparative Example 6

[0091] Take 50 grams of sucrose and 62.49 grams of sodium periodate, and the remaining steps and conditions are the same as those in Example 1. The aldehyde content of the dibasic sugar-based cross-linking agent prepared by this method is 6.03 mmol / g.

[0092] Comparative Example 5

[0093] Take 50 grams of sucrose and 89.35 grams of sodium periodate, and the remaining steps and conditions are the same as those in Example 1. The dibasic sugar-based cross-linking agent prepared by this method has an aldehyde content of 12.11 mmol / g.

[0094] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a dibasic sugar-based cross-linking agent, characterized in that: The following steps are involved: (1) dissolving a dibasic sugar in a weakly polar organic solvent, stirring and dissolving to obtain a dibasic sugar organic solution, dissolving a periodate in distilled water, stirring and dissolving in a light-proof condition to obtain a periodate aqueous solution; (2) lowering the temperature of the disaccharide organic solution prepared in step (1) to room temperature, and dripping a light-shielded periodate aqueous solution into the disaccharide organic solvent to react under the condition of shielding from light and introducing protective gas; (3) After the reaction is completed, the reaction solution is transferred to a -60°C to -20°C environment and frozen for 1 to 12 hours. Excess periodate and generated iodate are precipitated in the form of salt. The salt is recovered by vacuum filtration to obtain a mother solution of a diglycosyl cross-linking agent, which is then stored at -60°C to -20°C for future use. (4) drying the mother solution of the diglycosyl crosslinking agent under reduced pressure at -60 to -50°C and a pressure of 4 Pa ​​for 6 to 8 hours to obtain a water-free and organic solvent-free powder, namely the diglycosyl crosslinking agent; The weakly polar organic solvent in step (1) is at least one of N,N-dimethylformamide, N,N-dimethylacetamide and dimethyl sulfoxide.

2. The method for preparing a dibasic sugar-based cross-linking agent according to claim 1, characterized in that: The disaccharide in step (1) is sucrose or maltose; the concentration of the disaccharide in the disaccharide organic solution is 0.05-0.15 g / ml.

3. The method for preparing a dibasic sugar-based cross-linking agent according to claim 1, characterized in that: The periodate in step (1) is at least one of sodium periodate and potassium periodate; and the concentration of periodate in the periodate aqueous solution is 0.2-0.3 g / ml.

4. The method for preparing a dibasic sugar-based cross-linking agent according to claim 1, characterized in that: The molar ratio of periodate to dibasic sugar in step (1) is 3.2-4.5:

1.

5. The method for preparing a dibasic sugar-based cross-linking agent according to claim 1, characterized in that: The protective gas in step (2) is nitrogen or helium.

6. The method for preparing a dibasic sugar-based cross-linking agent according to claim 1, characterized in that: The dropping speed in step (2) is 20 ml / min.

7. The method for preparing a dibasic sugar-based cross-linking agent according to claim 1, characterized in that: The light-proof reaction temperature in step (2) is 5-15° C., and the light-proof reaction time is 30 minutes to 3 hours.

8. A method for processing wrinkle-resistant fabrics using the dibasic sugar-based crosslinking agent prepared according to claim 1, characterized in that: The following steps are involved: S1. Preparation of working solution: adding 0.5-5 g / L whiteness or color protection agent and catalyst to the mother solution of the diglycosyl crosslinking agent, and then adding an alkali agent to adjust the pH value of the mother solution to 2-5; adding a solvent to obtain a solution with an effective content of 5-8% of the diglycosyl crosslinking agent; S2, application of crosslinking agent: immersing the fabric in the solution of step S1 by two dipping and two rolling, with the fabric carrying 90-110% of the solution, and then performing a crosslinking reaction; S3, impurity removal and washing: put the baked fabric into a solution of 0.5-1g / L soap flakes and 0.1-2g / L sodium carbonate, with a bath ratio of 5:1, and wash at 40-60°C for 5-10 minutes; The catalyst is formic acid, and the amount of the catalyst added is 0.1-1 g / L; The alkali agent is sodium carbonate or sodium bicarbonate; The solvent is water or a weakly polar organic solvent.

9. The method for processing wrinkle-resistant fabric according to claim 8, characterized in that: The whiteness or color protection agent described in step S1 is N-methylformamide or formamide; The weakly polar organic solvent is any one or more of N,N-dimethylformamide, N,N-dimethylacetamide and dimethyl sulfoxide.

10. The method for processing anti-wrinkle fabric according to claim 8, characterized in that: The cross-linking reaction process conditions described in step S2 are: pre-baking at 110-130° C. for 10-30 seconds and baking at 150-180° C. for 60 seconds to 300 seconds.

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