Preparation method of cool ammonia cotton fabric
By preparing silicone polyurethane finishing agent and sorting the ammonia cotton fabric, the problem of poor wrinkle and pilling resistance of ammonia cotton fabric is solved, and a higher feel level, wrinkle recovery angle and pilling resistance are achieved, while maintaining high revitalization rate and hydrophilic and hygroscopic properties.
Patent Information
- Application Number
- CN202510284488.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-11
- Publication Date
- 2025-06-06
AI Technical Summary
The existing ammonia cotton fabrics have poor performance in wrinkle resistance and pill resistance, and their softness and coolness are not ideal.
The polyether polyol and isocyanate compound were reacted in a nitrogen atmosphere, tetrahydrofuran and silicone aqueous chain extender were added to prepare silicone polyurethane finishing agent, and the ammonia cotton fabric was sorted through the two-thimmersion and two-roll finishing method.
It improves the soft feel, wrinkle resistance and pilling performance of ammonia cotton fabric, improves the feel level, wrinkle recovery angle and pilling resistance, while maintaining high revitalization and hydrophilic and hygroscopic properties.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of fabrics, in particular to a method for preparing a cool spandex fabric. Background Art
[0002] Cotton fabrics have excellent breathability, moisture absorption, warmth retention, heat resistance and other properties, and are widely used. Blending cotton fibers with spandex, polyester, etc. can produce fabrics with better performance. Among them, spandex-cotton fabrics are textile fabrics made of spandex fibers and cotton fibers, which have excellent breathability, moisture absorption, high elastic recovery, and wear resistance. Traditional cotton fabrics and their blended fabrics have problems such as easy pilling.
[0003] In order to further improve the anti-wrinkle, anti-pilling, soft and cool feel of fabrics, it is necessary to use finishing agents to finish the fabrics. Common finishing agents include polyurethane finishing agents, silicone oil finishing agents, polyether finishing agents, etc. Chinese patent CN112281496B discloses a dyeing and finishing method for a cool imitation silk fabric of cotton spandex knitwear, using acrylic monomer, menthyl acetate, azobisisobutyronitrile, silicone oil, etc. as raw materials, preparing a cool softener containing a cool sustained-release agent, finishing the cotton spandex knitwear, so that the fabric has good gloss, drape, cool and soft touch, etc., but the patent does not improve the anti-wrinkle, anti-pilling and other properties of cotton spandex fabrics, and usually after finishing with silicone oil, the hydrophobicity of the fabric surface will increase, and the moisture regain and hygroscopicity will deteriorate. Summary of the invention
[0004] (I) Technical problems solved: In view of the deficiencies in the prior art, the present invention solves the problems of poor anti-wrinkle performance of spandex fabrics and poor hand feel such as softness and coolness.
[0005] (II) Technical solution: A method for preparing a cool spandex fabric:
[0006] (1) Dry and remove water from the polyether polyol, mix it with the isocyanate compound, react it at 75-80° C. for 2-2.5 hours in a nitrogen atmosphere, then add tetrahydrofuran, silicone water-based chain extender, and dibutyltin dilaurate, react it at 50-60° C. for 1-1.5 hours, distill it under reduced pressure, and dry it to obtain a silicone polyurethane finishing agent.
[0007] (2) Adding a silicone polyurethane finishing agent and an emulsifier to water, stirring, and then adding ammonia cotton fabric, the bath ratio is 40:1, and performing two-immersion and two-rolling finishing, then taking out the fabric, washing and drying, to obtain a cool-feeling ammonia cotton fabric.
[0008] Preferably, the amount of polyether polyol used is 100 parts by weight, the isocyanate compound is 20-27 parts by weight, the organic silicone water-based chain extender is 16-19 parts by weight, and the amount of dibutyltin dilaurate is 0.06-0.09 parts by weight.
[0009] Preferably, the polyether polyol is polyethylene glycol 2000 or polypropylene glycol 2000.
[0010] Preferably, the isocyanate compound is hexamethylene diisocyanate or isophorone diisocyanate.
[0011] Preferably, the preparation method of the organic silicon water-based chain extender is: tetrahydrofuran, 100 parts by weight of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane (CAS registration number 2469-55-8), 156-164 parts by weight of 4-(2-oxiranylmethoxy)benzoic acid (CAS registration number 35217-95-9) are mixed, reacted at 40-50°C for 5-7h, distilled under reduced pressure, washed with methanol, and the product is recrystallized in dichloromethane to obtain the organic silicon water-based chain extender. The reaction formula is:
[0012]
[0013] Preferably, (2) the amount of water used is 100 parts by weight, the amount of the silicone polyurethane finishing agent is 2-6 parts by weight, and the amount of the emulsifier is 0.03-0.08 parts by weight.
[0014] (III) Technical effect: The present invention uses diols such as polyethylene glycol, isocyanate compounds such as isophorone diisocyanate, and water-based silicone chain extenders containing hydroxyl and imino groups as raw materials to prepare a new type of silicone polyurethane finishing agent. The finishing agent contains a flexible siloxane structure, which can improve the soft feel, wrinkle resistance and anti-pilling performance of the spandex cotton fabric, and has a higher hand feel grade, wrinkle recovery angle and anti-pilling grade. The silicone polyurethane finishing agent contains hydrophilic carboxyl groups, which can keep the spandex cotton fabric at a high moisture regain and hydrophilic moisture absorption performance, and at the same time make the fabric have a hydrophilic and cool feel. DETAILED DESCRIPTION
[0015] The emulsifier model is AY3320, Anyi Chemical (Jiangsu) Co., Ltd. Spandex fabric, 95% cotton fiber, 5% spandex fiber.
[0016] Example 1
[0017] (1) 8 mL of tetrahydrofuran, 5 g of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, and 7.8 g of 4-(2-oxiranylmethoxy)benzoic acid were mixed, reacted at 50° C. for 5 h, distilled under reduced pressure, washed with methanol, and the product was recrystallized in dichloromethane to obtain an organic silicone water-based chain extender.
[0018] (2) 100 g of polyethylene glycol 2000 was dried and dehydrated, mixed with 27 g of isophorone diisocyanate, reacted at 75° C. for 2 h in a nitrogen atmosphere, then 70 mL of tetrahydrofuran, 17 g of an organic silicone water-based chain extender, and 0.08 g of dibutyltin dilaurate were added, reacted at 55° C. for 1.5 h, and distilled under reduced pressure and dried to obtain an organic silicone polyurethane finishing agent.
[0019] (3) Add 200 g of silicone polyurethane finishing agent and 3 g of emulsifier to 10 L of water, stir and add ammonia cotton fabric, the bath ratio is 40:1, and perform double immersion and double rolling finishing with a rolling rate of 85%. Then take out the fabric, wash it with water, pre-bake it at 80°C for 5 min, and bake it at 160°C for 3 min to obtain a cool ammonia cotton fabric.
[0020] Example 2
[0021] (1) 100 mL of tetrahydrofuran, 5 g of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, and 8.2 g of 4-(2-oxiranylmethoxy)benzoic acid were mixed, reacted at 40° C. for 7 h, distilled under reduced pressure, washed with methanol, and the product was recrystallized in dichloromethane to obtain an organic silicone water-based chain extender.
[0022] (2) 100 g of polypropylene glycol 2000 was dried and dehydrated, mixed with 26.4 g of isophorone diisocyanate, and reacted at 7° C. for 2.5 h in a nitrogen atmosphere, then 60 mL of tetrahydrofuran, 16.7 g of an organic silicone water-based chain extender, and 0.09 g of dibutyltin dilaurate were added, and the mixture was reacted at 60° C. for 1 h. The mixture was distilled under reduced pressure and dried to obtain an organic silicone polyurethane finishing agent.
[0023] (3) Add 300 g of silicone polyurethane finishing agent and 4.2 g of emulsifier to 10 L of water, stir and add ammonia cotton fabric, the bath ratio is 40:1, and perform double immersion and double rolling finishing, the rolling rate is 85%, then take out the fabric, wash it with water, pre-bake it at 80°C for 5 min, and bake it at 160°C for 3 min to obtain a cool ammonia cotton fabric.
[0024] Example 3
[0025] (1) 100 g of polypropylene glycol 2000 was dried and dehydrated, mixed with 20 g of hexamethylene diisocyanate, reacted at 80° C. for 2 h in a nitrogen atmosphere, then 60 mL of tetrahydrofuran, 16 g of an organic silicon water-based chain extender (prepared according to the method of Example 1), and 0.06 g of dibutyltin dilaurate were added, reacted at 50° C. for 1.5 h, and distilled under reduced pressure and dried to obtain an organic silicon polyurethane finishing agent.
[0026] (2) Add 400 g of silicone polyurethane finishing agent and 5.5 g of emulsifier to 10 L of water, stir and add ammonia cotton fabric, the bath ratio is 40:1, and perform double immersion and double rolling finishing, the rolling rate is 85%, then take out the fabric, wash it with water, pre-bake it at 80°C for 5 min, and bake it at 160°C for 3 min to obtain a cool ammonia cotton fabric.
[0027] Example 4
[0028] (1) 100 g of polyethylene glycol 2000 was dried and dehydrated, mixed with 27 g of isophorone diisocyanate, reacted at 75° C. for 2.5 h in a nitrogen atmosphere, then 80 mL of tetrahydrofuran, 19 g of an organic silicone water-based chain extender (prepared according to the method of Example 1), and 0.06 g of dibutyltin dilaurate were added, reacted at 60° C. for 1 h, and distilled under reduced pressure and dried to obtain an organic silicone polyurethane finishing agent.
[0029] (2) Add 500 g of silicone polyurethane finishing agent and 6.8 g of emulsifier to 10 L of water, stir and add ammonia cotton fabric, the bath ratio is 40:1, and perform double immersion and double rolling finishing, the rolling rate is 85%, then take out the fabric, wash it with water, pre-bake it at 80°C for 5 min, and bake it at 160°C for 3 min to obtain a cool ammonia cotton fabric.
[0030] Example 5
[0031] (1) 100 g of polyethylene glycol 2000 was dried and dehydrated, mixed with 22 g of hexamethylene diisocyanate, reacted at 75° C. for 2 h in a nitrogen atmosphere, then 60 mL of tetrahydrofuran, 16 g of an organic silicon water-based chain extender (prepared according to the method of Example 1), and 0.09 g of dibutyltin dilaurate were added, reacted at 50° C. for 1.5 h, and distilled under reduced pressure and dried to obtain an organic silicon polyurethane finishing agent.
[0032] (2) Add 600 g of silicone polyurethane finishing agent and 8 g of emulsifier to 10 L of water, stir and add ammonia cotton fabric, the bath ratio is 40:1, and perform double immersion and double rolling finishing, the rolling rate is 85%, then take out the fabric, wash it with water, pre-bake it at 80°C for 5 min, and bake it at 160°C for 3 min to obtain a cool ammonia cotton fabric.
[0033] Comparative Example 1 is an unfinished spandex fabric.
[0034] Comparative Example 2
[0035] (1) 100 g of polyethylene glycol 2000 was dried and dehydrated, mixed with 27 g of isophorone diisocyanate, reacted at 75° C. for 2 h in a nitrogen atmosphere, then 70 mL of tetrahydrofuran, 17 g of 2,2-dihydroxymethylpropionic acid, and 0.08 g of dibutyltin dilaurate were added, reacted at 55° C. for 1.5 h, and distilled under reduced pressure and dried to obtain a polyurethane finishing agent.
[0036] (2) Add 200 g of silicone polyurethane finishing agent and 3 g of emulsifier to 10 L of water, stir and add ammonia cotton fabric, the bath ratio is 40:1, and perform double immersion and double rolling finishing, the rolling rate is 85%, then take out the fabric, wash it with water, pre-bake it at 80°C for 5 min, and bake it at 160°C for 3 min to obtain a cool ammonia cotton fabric.
[0037] Comparative Example 3
[0038] (1) 100 g of polyethylene glycol 2000 was dried and dehydrated, mixed with 27 g of isophorone diisocyanate, reacted at 75° C. for 2 h in a nitrogen atmosphere, then 70 mL of tetrahydrofuran, 17 g of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane as a diamine chain extender, and 0.08 g of dibutyltin dilaurate were added, reacted at 55° C. for 1.5 h, and distilled under reduced pressure and dried to obtain a silicone polyurethane finishing agent.
[0039] (2) Add 200 g of silicone polyurethane finishing agent and 3 g of emulsifier to 10 L of water, stir and add ammonia cotton fabric, the bath ratio is 40:1, and perform double immersion and double rolling finishing, the rolling rate is 85%, then take out the fabric, wash it with water, pre-bake it at 80°C for 5 min, and bake it at 160°C for 3 min to obtain a cool ammonia cotton fabric.
[0040] An evaluation panel of 10 textile industry professionals evaluated the flexibility, coolness and feel of spandex fabrics by touch, with grades ranging from 1 to 5, with grade 1 being the worst and grade 5 being the best, and the average value was taken.
[0041] Test the wrinkle recovery angle (sum of warp and weft) of spandex fabric according to GB / T 3819-1997. Test the moisture regain of spandex fabric according to GB / T 9994-2018. Test the anti-pilling performance according to GB / T 4802.2-2008.
[0042] Table 1 Performance test of spandex fabric
[0043]
[0044] After testing, the unfinished spandex fabric of comparative example 1 had low hand feel ratings such as flexibility and coolness, low wrinkle recovery angle and anti-pilling grade, and poor anti-wrinkle and anti-pilling properties.
[0045] In Example 1-5, the spandex cotton fabric is finished with an organosilicon polyurethane finishing agent, which contains a flexible siloxane structure and can improve the soft feel, wrinkle resistance and anti-pilling performance of the spandex cotton fabric, and has a higher feel grade, wrinkle recovery angle and anti-pilling grade. In addition, the organosilicon polyurethane finishing agent contains a hydrophilic carboxyl group, which can make the spandex cotton fabric maintain a high moisture regain and hydrophilic moisture absorption performance, and at the same time make the fabric have a hydrophilic and cool feel.
[0046] Comparative Example 2 uses conventional 2,2-dimethylolpropionic acid as a water-based chain extender, and the prepared polyurethane finishing agent does not contain a flexible siloxane structure, the fabric has a poor hand feel rating, a low wrinkle recovery angle and anti-pilling grade, and poor anti-wrinkle and anti-pilling properties.
[0047] In Comparative Example 3, conventional 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is used as a diamine chain extender, and the prepared polyurethane finishing agent does not contain a hydrophilic carboxyl group, resulting in a significant decrease in the moisture regain of the cotton fabric and a deterioration in the hydrophilic moisture absorption performance.
Claims
1. A method for preparing a cool spandex fabric, characterized in that: The preparation method is: (1) drying and removing water from the polyether polyol, mixing with an isocyanate compound, reacting in a nitrogen atmosphere, then adding tetrahydrofuran, an organic silicon water-based chain extender, and dibutyltin dilaurate, distilling under reduced pressure after the reaction, and drying to obtain an organic silicon polyurethane finishing agent; (2) Adding an organosilicon polyurethane finishing agent and an emulsifier to water, stirring, and then adding ammonia cotton fabric to perform double dipping and double rolling finishing, then taking out the fabric, washing, and drying, to obtain a cool ammonia cotton fabric.
2. The method for preparing the cool spandex fabric according to claim 1, characterized in that: The polyether polyol is used in an amount of 100 parts by weight, the isocyanate compound is used in an amount of 20-27 parts by weight, the organic silicon water-based chain extender is used in an amount of 16-19 parts by weight, and the dibutyltin dilaurate is used in an amount of 0.06-0.09 parts by weight.
3. The method for preparing the cool spandex fabric according to claim 1, characterized in that: The polyether polyol is polyethylene glycol or polypropylene glycol.
4. The method for preparing the cool spandex fabric according to claim 2, characterized in that: The isocyanate compound is hexamethylene diisocyanate or isophorone diisocyanate.
5. The method for preparing the cool spandex fabric according to claim 1, characterized in that: The preparation method of the water-based organosilicon chain extender comprises: mixing tetrahydrofuran, 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane and 4-(2-oxiranylmethoxy)benzoic acid, reacting at 40-50° C. for 5-7 hours, distilling under reduced pressure, washing with methanol, and recrystallizing the product in dichloromethane to obtain the water-based organosilicon chain extender.
6. The method for preparing the cool spandex fabric according to claim 5, characterized in that: The amount of the 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane used is 100 parts by weight, and the amount of the 4-(2-oxiranylmethoxy)benzoic acid used is 156-164 parts by weight.
7. The method for preparing the cool spandex fabric according to claim 1, characterized in that: The temperature of the first reaction in (1) is 75-80°C, and the reaction time is 2-2.5h; the temperature of the second reaction is 50-60°C, and the reaction time is 1-1.5h.
8. The method for preparing the cool spandex fabric according to claim 1, characterized in that: The amount of (2) water is 100 parts by weight, the amount of the silicone polyurethane finishing agent is 2-6 parts by weight, and the amount of the emulsifier is 0.03-0.08 parts by weight.
Citation Information
Patent Citations
A dyeing and finishing method for a cool, silk-like cotton-spandex knitted fabric.
CN112281496B