CN112281493A - 一种无氟防水整理剂及其制备方法 - Google Patents
一种无氟防水整理剂及其制备方法 Download PDFInfo
- Publication number
- CN112281493A CN112281493A CN202011275846.8A CN202011275846A CN112281493A CN 112281493 A CN112281493 A CN 112281493A CN 202011275846 A CN202011275846 A CN 202011275846A CN 112281493 A CN112281493 A CN 112281493A
- Authority
- CN
- China
- Prior art keywords
- fluorine
- finishing agent
- free waterproof
- free
- waterproof finishing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 47
- -1 polysiloxane Polymers 0.000 claims abstract description 18
- IZHVBANLECCAGF-UHFFFAOYSA-N 2-hydroxy-3-(octadecanoyloxy)propyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)COC(=O)CCCCCCCCCCCCCCCCC IZHVBANLECCAGF-UHFFFAOYSA-N 0.000 claims abstract description 14
- OHJMTUPIZMNBFR-UHFFFAOYSA-N biuret Chemical compound NC(=O)NC(N)=O OHJMTUPIZMNBFR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 13
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 13
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims abstract description 7
- 229940074045 glyceryl distearate Drugs 0.000 claims abstract description 7
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940011051 isopropyl acetate Drugs 0.000 claims abstract description 7
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 claims abstract description 7
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 7
- 239000008234 soft water Substances 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000004744 fabric Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 9
- 239000005871 repellent Substances 0.000 claims description 9
- 230000001804 emulsifying effect Effects 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 229920000742 Cotton Polymers 0.000 claims description 7
- 230000002940 repellent Effects 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000004945 emulsification Methods 0.000 abstract description 8
- 150000002191 fatty alcohols Chemical class 0.000 abstract description 5
- QUSNBJAOOMFDIB-UHFFFAOYSA-N monoethyl amine Natural products CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 abstract 2
- 239000004094 surface-active agent Substances 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 1
- BAVYZALUXZFZLV-UHFFFAOYSA-N mono-methylamine Natural products NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 abstract 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229920004933 Terylene® Polymers 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 230000005183 environmental health Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 239000002939 oilproofing Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/165—Ethers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
- D06M13/2243—Mono-, di-, or triglycerides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/395—Isocyanates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/53—Polyethers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明提供一种无氟防水整理剂及其制备方法，包括二甘醇单丁醚10‑15％，醋酸异丙酯5‑10％，甲基烷基聚硅氧烷5‑10％，二硬脂酸甘油酯10‑15％，表面活性剂脂肪醇聚氧乙烯醚AEO6 5‑10％,甲基氨乙基胺丙基聚硅氧烷2‑10％，封端型缩二脲三异氰酸酯交联剂5‑10％，软水15‑50％。本发明的无氟防水整理剂生产方法简单，只需要一套高剪切的乳化设备，把上述原料二甘醇单丁醚、醋酸异丙酯、甲基烷基硅氧烷、二硬脂酸甘油酯、表面活性剂脂肪醇聚氧乙烯醚、甲基胺乙基胺丙基聚硅氧烷混在一起，然后高速剪切乳化，添加封端型缩二脲三异氰酸酯交联剂搅拌20分钟便得到乳白色粘稠无氟防水整理剂。
Description
技术领域
本发明涉及防水剂技术领域，尤其是一种无氟防水整理剂及其制备方法。
背景技术
纺织服装上的三防整理过去几十年都是以含全氟烷基为主，含有8个氟碳的防水防油剂(C8F17-)由于含有微量的PFOA或PFOS，这两种化学品对肝脏、神经、心血管系统、生殖系统和免疫系统等多种具有毒性和致癌性，PFOA和PFOS在体内持久性强，一旦摄取后，很难通过生物体的新陈代谢而分解，是最难分解的有机污染物，在任何环境下试验都没有出现水解、光解或生物降解现象，他们还有距离环境迁移能力，污染范围十分宽广。被国际健康与环境风险科学委员会确认是一类非常持久、生物积累和有毒的化学品。美国环境保护署(EPA)认为在织造和加工某些有机氟化学品时可释放出PFOA，包括生产PFOS时，以及全氟烷基调聚物和它的丙烯酸酯等共聚物在环境中分解时也会产生少量的PFOA,会在环境中聚集和在人体与动物组织中累积，对人体健康和生态环境产生潜在的危险。
近些年来，许多厂家已经停止生产长氟链的产品。从目前的替代物来看，新型6个氟碳的(C6F13-)含氟表面活性剂原料制造的整理剂具有最佳的替代性，然而仍存在着经济性和整体功能等问题，6个氟碳的(C6F13-)防水防油虽然毒性小于8个氟碳的防水防油剂(C8F17-)，生物降解性好于8个氟碳的防水防油剂(C8F17-)，但在生产过程中无组织排放和含氟整理剂的环境健康深入研究，未来应用前景并不乐观，只是一个过渡阶段的替代品。
这几年，许多国际知名服装和运动鞋品牌结成联盟，为了保护生态环境，逐渐放弃用含氟产品来做防水防油整理剂，甚至对防油效果不做要求。许多助剂厂商开始转向无氟防水整理剂的研究，是最近几年的研究热点。
发明内容
针对现有技术的不足，本发明提供一种无氟防水整理剂、及其制备方法，添加本发明的无氟防水整理剂织物，可提高其耐洗性，同时，可保证长时间不会发生交联、沉淀和漂浮物。
本发明的技术方案为：一种无氟防水整理剂，包括以下质量百分比的组分：
进一步的，所述的无氟防水整理剂包括以下质量百分比的组分：
进一步的，所述的无氟防水整理剂包括以下质量百分比的组分：
进一步的，所述的封端型缩二脲三异氰酸酯交联剂在高温焙烘下，能释放出-NCO反应性基团，与织物上的活性基、防水主要成分上的活性基发生化学反应，生成高分化合物或成网状结构，从而提高耐洗性。
本发明还提供一种无氟防水整理剂的制备方法，包括以下步骤，以下步骤的百分比为质量百分比：
S1)、在带有高速剪切装置的不锈钢反应釜里面先后分别注入10-15％的二甘醇单丁醚、5-10％醋酸异丙酯、5-10％甲基烷基聚硅氧烷、10-15％二硬脂酸甘油酯和10-15％的甲基氨乙基胺丙基聚硅氧烷充分混合，搅拌10-25min；
S2)、步骤S1)搅拌完成后，注入5-10％的脂肪醇聚氧乙烯醚AEO6，搅拌10-20分钟；开启高剪切乳化设备，慢慢注入15-50％的软水，乳化1-3小时，体系变成乳白色液体，停止乳化装置，开启普通搅拌装置，慢慢加入5-10％的封端型缩二脲三异氰酸酯交联剂，搅拌10-30分钟，得到乳白色粘稠无氟防水整理剂。
本发明还提供一种无氟防水整理剂的使用方法，
取本发明的无氟防水整理剂100-200g/L，在后整理定型机上使用，100℃烘干2-4min，180℃焙烘2-3min。经过本发明的无氟防水整理剂整理后的棉织物或化纤织物，防水等级能达到90分以上，经过5次洗水之后，防水等级仍具有80分以上。
进一步的，上述无氟防水整理剂在使用过程中，一浸一轧，带液率90-100％，织物浸轧前，保持布面不含有或少含有亲水类化学品，且布面pH为5.0-6.0。
本发明的有益效果为：
1、本发明的无氟整理剂因为含有热封端型缩二脲三异氰酸酯交联剂，整理在织物上，耐洗性可以提高不少于5次；且在室温条件下，比较稳定，不会发生交联反应；
2、本发明放置长时间都不会发生交联、沉淀和漂浮物，使用时，即使天气温度较高的条件下，定型机不会发生黏辊现象，使用稳定；
3、本发明的无氟防水主要采用酯类单体、含硅氧烷单体，这些单体复配，拒水效果稳定，色变小；
4、本发明的无氟防水整理剂含有封端型缩二脲三异氰酸酯交联剂，整理在织物上的耐洗性好，可以适合于纯棉织物和化纤织物，而且耐洗次数高，且本发明的无氟防水整理剂手感不会变差，在高温焙烘下；
5、经过本发明的无氟防水整理剂整理后的棉织物或化纤织物，防水等级能达到90分以上，经过5次洗水之后，防水等级仍具有80分以上；
具体实施方式
下面对本发明的具体实施方式作进一步说明：
实施例1
本实施例提供一种无氟防水整理剂的制备方法，包括以下步骤：
S1)、无氟防水整理剂配方：
S2)制备工艺：
在带有高速剪切装置的1000ml不锈钢反应釜里面先后分别注入100的g二甘醇单丁醚、50g醋酸异丙酯、50g甲基烷基聚硅氧烷、100g的二硬脂酸甘油酯和100g的甲基氨乙基胺丙基聚硅氧烷充分混合，搅拌20min之后，注入50g脂肪醇聚氧乙烯醚AEO6，搅拌15分钟，开启高剪切乳化设备，慢慢注入500g软水，乳化1小时，体系变成乳白色液体，停止乳化装置，开启普通搅拌装置，慢慢加入封端型缩二脲三异氰酸酯交联剂50g，搅拌20分钟，得到氟防水整理剂。
实施例2
本实施例提供一种无氟防水整理剂的制备方法，包括以下步骤：
S1)、无氟防水整理剂配方：
S2)、制备工艺：
在带有高速剪切装置的1000ml不锈钢反应釜里面先后分别注入二甘醇单丁醚125g、醋酸异丙酯75g、甲基烷基聚硅氧烷75g、二硬脂酸甘油酯125g和甲基氨乙基胺丙基聚硅氧烷125g充分混合，搅拌20min之后，注入75g脂肪醇聚氧乙烯醚AEO6，搅拌15分钟，开启高剪切乳化设备，慢慢注入325g软水，乳化1小时，体系变成乳白色液体，停止乳化装置，开启普通搅拌装置，慢慢加入封端型缩二脲三异氰酸酯交联剂75g，搅拌20分钟，即得氟防水整理剂。
实施例3
施例提供一种无氟防水整理剂的制备方法，包括以下步骤：
S1)、无氟防水整理剂配方：
S2)、制备工艺
在带有高速剪切装置的1000ml不锈钢反应釜里面先后分别注入二甘醇单丁醚150g、醋酸异丙酯100g、甲基烷基聚硅氧烷100g、二硬脂酸甘油酯150g和甲基氨乙基胺丙基聚硅氧烷20g充分混合，搅拌20min之后，注入100g脂肪醇聚氧乙烯醚AEO6，搅拌15分钟，开启高剪切乳化设备，慢慢注入150软水，乳化1小时，体系变成乳白色液体，停止乳化装置，开启普通搅拌装置，慢慢加入封端型缩二脲三异氰酸酯交联剂100g，搅拌20分钟，得到氟防水整理剂。
实施例4
应用与效果测试
纺织面料：涤纶针织物，纯棉针织物
整理液配制：
实施例1或实施例2或实施例3 100-200g
软化水 若干
共计 1000g
用醋酸调节PH至5-6之间，搅拌均匀
整理工艺：将织物浸泡在整理液中，一浸一轧(轧余率90-100％)，然后100℃烘干3分钟，在180℃焙烘3分钟。
拒水测试：对织物的拒水级别测试，一般用淋水性能测试方法，参考AATCC22-1977实验方法。
洗水方法：采用模拟洗衣机机洗方法，2g/L市售洗衣粉，浴比1:50，室温洗X25min为1次，反复洗5次。
白度测试：测试整理织物前后的白度指数，采用温州仪器厂生产的SBD型白度仪测试，测试结构如表1所示。
表1实施例防水整理效果及耐洗性
从表测试结果，实施例1,2,3都有很好的拒水效果，没有经过水洗，用量100g/L在纯棉和涤纶上都能达到90分，经过5次洗水之后，仍能达到80分以上，其中实施例3的耐洗牢度比较好，能达到85分；用量200g/L在纯棉和涤纶上都能达到100分，经过5次洗水之后，实施例1,2,3都能达到90分。用量加大，实施例1,2,3拒水效果和耐洗性无明显差别，都很好。
上述实施例和说明书中描述的只是说明本发明的原理和最佳实施例，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。
Claims (6)
1.一种无氟防水整理剂，其特征在于，包括以下质量百分比的组分：
所述的封端型缩二脲三异氰酸酯交联剂在高温焙烘下，能释放出-NCO反应性基团，与织物上的活性基、防水主要成分上的活性基发生化学反应，生成高分化合物或成网状结构，从而提高耐洗性。
2.根据权利要求1所述的一种无氟防水整理剂，其特征在于：所述的无氟防水整理剂包括以下质量百分比的组分：
所述的封端型缩二脲三异氰酸酯交联剂在高温焙烘下，能释放出-NCO反应性基团，与织物上的活性基、防水主要成分上的活性基发生化学反应，生成高分化合物或成网状结构，从而提高耐洗性。
3.根据权利要求1所述的一种无氟防水整理剂，其特征在于：所述的无氟防水整理剂包括以下质量百分比的组分：
所述的封端型缩二脲三异氰酸酯交联剂在高温焙烘下，能释放出-NCO反应性基团，与织物上的活性基、防水主要成分上的活性基发生化学反应，生成高分化合物或成网状结构，从而提高耐洗性。
4.一种用于制备权利要求1-3任一项所述的无氟防水整理剂的方法，其特征在于：以下步骤的百分比为质量百分比：
S1)、在带有高速剪切装置的不锈钢反应釜里面先后分别注入10-15％的二甘醇单丁醚、5-10％醋酸异丙酯、5-10％甲基烷基聚硅氧烷、10-15％二硬脂酸甘油酯和10-15％的甲基氨乙基胺丙基聚硅氧烷充分混合，搅拌10-25min；
S2)、步骤S1)搅拌完成后，注入5-10％的脂肪醇聚氧乙烯醚AEO6，搅拌10-20分钟；开启高剪切乳化设备，慢慢注入15-50％的软水，乳化1-3小时，体系变成乳白色液体，停止乳化装置，开启普通搅拌装置，慢慢加入5-10％的封端型缩二脲三异氰酸酯交联剂，搅拌10-30分钟，得到乳白色粘稠无氟防水整理剂。
5.一种使用权利要求1-4任一项所述的无氟防水整理剂的方法，其特征在于：
取上述的无氟防水整理剂100-200g/L，在后整理定型机上使用，100℃烘干2-4min，180℃焙烘2-3min，经过无氟防水整理剂整理后的棉织物或化纤织物，防水等级能达到90分以上，经过5次洗水之后，防水等级仍具有80分以上。
6.根据权利要求5所述的无氟防水整理剂的使用方法：其特征在于：
上述无氟防水整理剂在使用过程中，一浸一轧，带液率90-100％，织物浸轧前，保持布面不含有或少含有亲水类化学品，且布面pH为5.0-6.0。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011275846.8A CN112281493A (zh) | 2020-11-16 | 2020-11-16 | 一种无氟防水整理剂及其制备方法 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011275846.8A CN112281493A (zh) | 2020-11-16 | 2020-11-16 | 一种无氟防水整理剂及其制备方法 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112281493A true CN112281493A (zh) | 2021-01-29 |
Family
ID=74398865
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011275846.8A Pending CN112281493A (zh) | 2020-11-16 | 2020-11-16 | 一种无氟防水整理剂及其制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112281493A (zh) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113529423A (zh) * | 2021-06-09 | 2021-10-22 | 五邑大学 | 有机硅拒水剂、纸尿裤面层疏水喷涂处理工艺及纸尿裤 |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3933756A (en) * | 1972-08-05 | 1976-01-20 | Bayer Aktiengesellschaft | Process of preparation of synthetic resins by reacting a cross-linked isocyanate polyaddition product with low molecular weight polyisocyanate followed by reaction with an amino alkyl silane |
| CN102154834A (zh) * | 2010-12-17 | 2011-08-17 | 湖南大学 | 超疏水纤维、织物的简易制备方法及用途 |
| US20150086713A1 (en) * | 2013-09-23 | 2015-03-26 | Tamkang University | Non-fluoro hydrophobic aqueous-based polyurethane resin dispersion, and production method and use thereof |
| CN105037679A (zh) * | 2015-09-23 | 2015-11-11 | 苏州依司特新材料科技有限公司 | 阳离子型聚氨酯改性有机硅拒水剂及其制备方法与应用 |
| CN105646884A (zh) * | 2016-03-22 | 2016-06-08 | 中科院广州化学有限公司南雄材料生产基地 | 一种多羟基聚硅氧烷及耐磨超疏水涂层及制备方法 |
| CN105671967A (zh) * | 2016-03-16 | 2016-06-15 | 广州恒锦化工科技有限公司 | 一种持久性无氟防水剂及其制备方法 |
| CN106049069A (zh) * | 2016-07-15 | 2016-10-26 | 北京理工大学 | 一种具有支化结构无氟织物拒水剂及其制备方法 |
| CN106480741A (zh) * | 2016-09-22 | 2017-03-08 | 广州大学 | 一种多功能纺织品的整理方法 |
| CN110042661A (zh) * | 2019-03-22 | 2019-07-23 | 东莞东阳光科研发有限公司 | 整理剂组合物、整理剂及其制备方法和应用 |
| CN110409183A (zh) * | 2019-08-31 | 2019-11-05 | 三赢家居用品(河源)有限公司 | 一种无氟防水整理剂及其制备和应用方法 |
| CN110452361A (zh) * | 2019-07-09 | 2019-11-15 | 广东德美精细化工集团股份有限公司 | 一种聚氨酯丙烯酸改性有机硅无氟防水剂的合成方法及防水剂 |
-
2020
- 2020-11-16 CN CN202011275846.8A patent/CN112281493A/zh active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3933756A (en) * | 1972-08-05 | 1976-01-20 | Bayer Aktiengesellschaft | Process of preparation of synthetic resins by reacting a cross-linked isocyanate polyaddition product with low molecular weight polyisocyanate followed by reaction with an amino alkyl silane |
| CN102154834A (zh) * | 2010-12-17 | 2011-08-17 | 湖南大学 | 超疏水纤维、织物的简易制备方法及用途 |
| US20150086713A1 (en) * | 2013-09-23 | 2015-03-26 | Tamkang University | Non-fluoro hydrophobic aqueous-based polyurethane resin dispersion, and production method and use thereof |
| CN105037679A (zh) * | 2015-09-23 | 2015-11-11 | 苏州依司特新材料科技有限公司 | 阳离子型聚氨酯改性有机硅拒水剂及其制备方法与应用 |
| CN105671967A (zh) * | 2016-03-16 | 2016-06-15 | 广州恒锦化工科技有限公司 | 一种持久性无氟防水剂及其制备方法 |
| CN105646884A (zh) * | 2016-03-22 | 2016-06-08 | 中科院广州化学有限公司南雄材料生产基地 | 一种多羟基聚硅氧烷及耐磨超疏水涂层及制备方法 |
| CN106049069A (zh) * | 2016-07-15 | 2016-10-26 | 北京理工大学 | 一种具有支化结构无氟织物拒水剂及其制备方法 |
| CN106480741A (zh) * | 2016-09-22 | 2017-03-08 | 广州大学 | 一种多功能纺织品的整理方法 |
| CN110042661A (zh) * | 2019-03-22 | 2019-07-23 | 东莞东阳光科研发有限公司 | 整理剂组合物、整理剂及其制备方法和应用 |
| CN110452361A (zh) * | 2019-07-09 | 2019-11-15 | 广东德美精细化工集团股份有限公司 | 一种聚氨酯丙烯酸改性有机硅无氟防水剂的合成方法及防水剂 |
| CN110409183A (zh) * | 2019-08-31 | 2019-11-05 | 三赢家居用品(河源)有限公司 | 一种无氟防水整理剂及其制备和应用方法 |
Non-Patent Citations (1)
| Title |
|---|
| 马建中 等: "《皮革化学品》", 31 March 2008, 化学工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113529423A (zh) * | 2021-06-09 | 2021-10-22 | 五邑大学 | 有机硅拒水剂、纸尿裤面层疏水喷涂处理工艺及纸尿裤 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5883185A (en) | Water soluble fiber-treating agent and method of making | |
| CA1085563A (en) | Textile treating compositions | |
| CN104179013B (zh) | 防水防油剂组合物及防水防油剂添加剂组合物 | |
| KR100999334B1 (ko) | 아미노실록산 수중유형 에멀전 | |
| US20020132952A1 (en) | Water-soluble, water/oil repellent treating composition and method of making | |
| WO2009064503A1 (en) | Fabric treatment process | |
| JP2020503394A (ja) | 非フッ素化コーティング及び仕上げ剤 | |
| US4560487A (en) | Blends of fluorochemicals and fibrous substrates treated therewith | |
| WO2014184097A1 (de) | Wasserabweisende effekte auf textilen oberflächen | |
| EP0709517B1 (en) | Process for imparting oil- and water-repellency to textile fibres, skin, leather | |
| CN112281493A (zh) | 一种无氟防水整理剂及其制备方法 | |
| US20110015332A1 (en) | Oil-in-water aminosiloxane emulsions | |
| DE10259291B4 (de) | Hochkonzentrierte, selbstemulgierende Zubereitungen, enthaltend Organopolysiloxane und Alkylammoniumverbindungen und deren Verwendung in wässrigen Systemen | |
| CN109056320B (zh) | 一种基于棉织物的阻燃疏水整理方法 | |
| CN105088800A (zh) | 一种低温水性防水剂及其生产工艺 | |
| CN112030551B (zh) | 一种有机硅无氟防水柔软的涤纶基拉舍尔毛毯整理工艺 | |
| DE102005056864B4 (de) | Zubereitungen auf Basis von ammonium- und polyethermodifizierten Organopolysiloxanen und deren Verwendung zur Veredlung textiler Substrate | |
| CN114206959A (zh) | 丙烯酸酯低聚物、丙烯酸酯低聚物乳液和包含上述物质的无氟去污性组合物 | |
| DE19835227A1 (de) | Wäßrige Mikroemulsionen, enthaltend Organopolysiloxane | |
| US3476583A (en) | Method for rendering fibrous material oil and water repellent | |
| CN113430681B (zh) | 腈纶原液着色丝油剂 | |
| JP2613562B2 (ja) | 浸透剤 | |
| EP2196528B1 (en) | Fabric treating composition, detergent and softener, and treatment of fabric articles | |
| CN111434847A (zh) | 一种亲水易去污织物 | |
| CN110735325B (zh) | 一种改性环氧基poss无氟防水整理剂及其制备方法 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220222 Address after: 528000 F5, No. 3-1, Kaiyuan Road, Datang Park, Sanshui Industrial Park, Foshan City, Guangdong Province Applicant after: Guangdong Jusheng New Material Technology Co.,Ltd. Address before: No. 22, Dongcheng village, Jiangmen City, Guangdong Province Applicant before: WUYI University |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210129 |