WO2021004369A1 - 一种绿色环保型浸胶液及其生产方法 - Google Patents

一种绿色环保型浸胶液及其生产方法 Download PDF

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WO2021004369A1
WO2021004369A1 PCT/CN2020/099960 CN2020099960W WO2021004369A1 WO 2021004369 A1 WO2021004369 A1 WO 2021004369A1 CN 2020099960 W CN2020099960 W CN 2020099960W WO 2021004369 A1 WO2021004369 A1 WO 2021004369A1
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Prior art keywords
dipping liquid
green
composition
environmentally friendly
latex
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PCT/CN2020/099960
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English (en)
French (fr)
Inventor
王志强
姜广峰
赵建平
刘一东麟
王飞
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蔚林新材料科技股份有限公司
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Priority to US17/597,369 priority Critical patent/US20220235210A1/en
Priority to EP20836181.6A priority patent/EP3978679A4/en
Publication of WO2021004369A1 publication Critical patent/WO2021004369A1/zh

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    • C08L9/06—Copolymers with styrene
    • C08L9/08—Latex
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
    • B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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Definitions

  • the invention relates to the technical field of dipping preparation, in particular to an environmentally friendly green dipping solution containing no formaldehyde and resorcinol and a production method thereof.
  • the raw materials such as resorcinol and ammonia in the RFL system have foul and pungent odors, and the preparation workshop is prone to produce peculiar smell; and formaldehyde solution, as a dangerous chemical, has higher safety management requirements during storage and use, which improves the The explosion-proof grade of the glue preparation workshop.
  • the impregnant currently used by Goodyear is mainly composed of one or two acrylic monomers and a small amount of styrene to prepare an acrylic resin, and the acrylic resin is mixed with latex to make an impregnation formula.
  • the acrylic resin is mixed with latex to make an impregnation formula.
  • two-bath acrylic resin-latex system dipping is completed in two steps.
  • the performance of the skeleton material after dipping is close to that of the traditional RFL system.
  • the overall process is complicated, the equipment investment is high, and the raw materials are all its designated suppliers, and the dependence on upstream products is high.
  • the current patent-protected formula of Pirelli Tire Co., Ltd. contains at least rubber latex, epoxy compounds and polyamines with a molecular weight greater than 190 Daltons.
  • the viscosity of these compositions between the frame material and the rubber compound is close to that of the traditional RFL system used in the industry.
  • the polyamine raw materials used in the formula are demanding and the purchase cost is high.
  • the use of polyamine raw materials in the traditional production workshop does not conform to the current environmental protection policy, and it is easy to stick to the hub during the dipping process, which is not conducive to the phased shutdown and maintenance. Unfavorable factors such as continuous production.
  • the technical problem to be solved by the present invention is: in view of the technical problems existing in the above-mentioned dipping liquid, the present invention provides a green and environment-friendly dipping liquid and a production method thereof.
  • the dipping liquid of the invention does not contain toxic and harmful substances such as formaldehyde and resorcinol, and the production method is simple and easy to operate, the production cycle is short, and the safety factor is high, and the preparation of the dipping liquid and the safe and green production of the dipping process are realized.
  • the present invention provides a green and environmentally friendly dipping liquid, expressed in weight percentage, the raw material composition of the green and environmentally friendly dipping liquid is: blocked isocyanate 1-15%, special amino resin 0.5-10%, rubber latex 10-50%, auxiliaries 1-5%, the rest is water, the total weight percentage of each component is 100%;
  • the auxiliary agent is composed of auxiliary agent a and auxiliary agent b, and the mass ratio between the two is 1:1-3.
  • the raw material composition of the green environmentally friendly dipping liquid is: 1 to 5% of blocked isocyanate, 1.5 to 10% of special amino resin, and 20 to 20 of rubber latex. 40%, additives 3 to 5%, the rest is water, and the total weight percentage of each component is 100%;
  • the auxiliary agent is composed of auxiliary agent a and auxiliary agent b, and the mass ratio between the two is 1:1-3.
  • the special amino resin is one or more of urea-formaldehyde resin, melamine-formaldehyde resin, benzoxazine resin and polyamide polyamine epichlorohydrin.
  • the rubber latex is pyridine butadiene latex, butadiene latex, EPDM, styrene butadiene latex, natural rubber latex, nitrile butadiene latex, carboxyl butadiene butadiene rubber latex, and carboxyl styrene butadiene latex. And one or more of carboxyl nitrile latex.
  • the auxiliary agent a is Tween-20, sodium diisobutylnaphthalene sulfonate, Tween 80 or fatty alcohol polyoxyethylene ether.
  • the auxiliary agent b is a high-granularity kaolin china clay wet superfine grinding auxiliary agent, an aqueous calcium stearate emulsion or sodium hexametaphosphate.
  • the solid content of the dipping liquid is 5-30%.
  • the production method includes the following steps:
  • composition 1 b. Add the weighed blocked isocyanate and auxiliary a to water and stir evenly to obtain composition 1;
  • the solid particle size distribution in the composition 3 after grinding in step d is 1-50 ⁇ m.
  • the dipping liquid of the present invention is formed by providing one or more forces between the organic fiber material and the rubber to make the organic fiber material and the rubber adhere to each other; the dipping liquid of the present invention uses blocked isocyanate and special amino resin It does not contain toxic and harmful substances such as formaldehyde and resorcinol; its production method is simple and easy to operate, short production cycle and high safety factor. In this way, safe and green production of the dipping liquid preparation and dipping process is realized, and there is no waste generation in the entire production process, which is environmentally friendly.
  • the dipping liquid of the present invention is different from the original RFL dipping liquid for ready-to-use, the dipping liquid can be stably stored and transported, filling the gap in the current commodity market.
  • Fig. 1 is a schematic diagram of the process flow of the preparation method of the green and environment-friendly dipping liquid of the present invention.
  • the raw materials used are all commercially available products, of which:
  • Blocked isocyanate its viscosity: 200-500mpa.s/25°C, solid content 50 ⁇ 1.5%, density: 1.0 ⁇ 0.2g/cm 3 (20°C), particle size, ⁇ 5 ⁇ m;
  • Bisphenol A/aniline benzoxazine resin MW is 466-800, softening point is 50-90°C, gel time (210°C, 1g) is 100-400 seconds;
  • Phenol/MDA type benzoxazine resin MW is 438-800, softening point is 50-90°C, gel time (210°C, 1g) is 100-400 seconds;
  • Bisphenol F/aniline benzoxazine resin MW is 438-800, softening point is 50-90°C, gel time (210°C, 1g) is 100-400 seconds;
  • Butadiene pyridine latex viscosity is 20-45mpa.s/25°C, solid content is 39.5-41.5%, density: 0.980-0.990g/cm 3 (20°C), pH is 10-12;
  • Carboxyl styrene butadiene latex viscosity is 4-350mpa.s/25°C, solid content is 48.0-54.0%, density: 0.970-0.100g/cm 3 (20°C), pH is 7.0-9.0;
  • Styrene-butadiene latex Viscosity is 200-800mpa.s/25°C, solid content is 48.0-61.0%, density: 0.960-0.980g/cm 3 (20°C), pH is 8.0-10.5;
  • Butadiene latex viscosity is 10-50mpa.s/25°C, solid content is 48.0-54.0%, density: 1.01-1.20g/cm 3 (20°C), pH is 12.0-14.0;
  • Nitrile latex its viscosity is 7-50mpa.s/25°C, solid content is 43.0-45.0%, pH is 7.0-8.0;
  • the carboxyl styrene butadiene latex has a viscosity of 4-350mpa.s/25°C, a solid content of 48.0-54.0%, a density of 0.970-0.100g/cm 3 (20°C), and a pH of 7.0-9.0.
  • the green and environment-friendly dipping liquid of the present invention is expressed in weight percentage. Its raw material composition is: 150kg of blocked isocyanate, 5kg of benzoxazine resin, 100kg of butadiene pyridine latex, and 15kg of auxiliary a (fatty alcohol polyoxyethylene ether) , Adjuvant b (sodium hexametaphosphate) 25kg, softened water 705kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 15.0%.
  • a benzoxazine resin with a bisphenol A/aniline bicyclic structure ie, bisphenol A/aniline benzoxazine resin
  • the green and environment-friendly dipping liquid of the present invention is expressed in percentage by weight. Its raw material composition is: 100kg of blocked isocyanate, 15kg of benzoxazine resin, 300kg of carboxyl styrene butadiene latex, and auxiliary a (fatty alcohol polyoxyethylene ether) 15kg, additive b (sodium hexametaphosphate) 25kg, softened water 545kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 24%.
  • This embodiment uses a phenol/MDA bicyclic benzoxazine resin (ie, a phenol/MDA type benzoxazine resin).
  • the green and environment-friendly dipping liquid of the present invention is expressed in weight percentage, and its raw material composition is: 50kg of blocked isocyanate, 15kg of benzoxazine resin, 300kg of butadiene pyridine latex, and 15kg of auxiliary a (fatty alcohol polyoxyethylene ether) , Additive b (sodium hexametaphosphate) 25kg, softened water 595kg, the total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 18.0%.
  • This embodiment uses a bisphenol F/MDA bicyclic benzoxazine resin (ie, bisphenol F/aniline benzoxazine resin).
  • the green and environment-friendly dipping liquid of the present invention is expressed in weight percentage, and its raw material composition is: 50kg of blocked isocyanate, 60kg of benzoxazine resin, 500kg of carboxyl styrene butadiene latex, and auxiliary a (fatty alcohol polyoxyethylene ether) 15kg, additives b (sodium hexametaphosphate) 25kg, softened water 350kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 35.5%.
  • This embodiment uses a bisphenol F/MDA bicyclic benzoxazine resin (ie, bisphenol F/aniline benzoxazine resin).
  • the green and environment-friendly dipping liquid of the present invention is expressed in weight percentage, and its raw material composition is: 10kg of blocked isocyanate, 100kg of benzoxazine resin, 300kg of carboxyl styrene butadiene latex, and auxiliary a (fatty alcohol polyoxyethylene ether) 15kg, additive b (sodium hexametaphosphate) 25kg, softened water 550kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 30%.
  • a benzoxazine resin with a bisphenol A/aniline bicyclic structure ie, bisphenol A/aniline benzoxazine resin
  • the green environmental protection dipping liquid of the present invention is expressed in weight percentage, and its raw material composition is: 150kg of blocked isocyanate, 5kg of benzoxazine resin, 100kg of EPDM rubber, and auxiliary a (fatty alcohol polyoxyethylene ether) ) 15kg, adjuvant b (sodium hexametaphosphate) 25kg, softened water 705kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 15.0%.
  • a benzoxazine resin with a bisphenol A/aniline bicyclic structure ie, bisphenol A/aniline benzoxazine resin
  • the green environmental protection type dipping liquid of the present invention is expressed in weight percentage, and its raw material composition is: 100kg of blocked isocyanate, 15kg of benzoxazine resin, 300kg of EPDM rubber, and auxiliary a (fatty alcohol polyoxyethylene ether) ) 15kg, adjuvant b (sodium hexametaphosphate) 25kg, softened water 545kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 24%.
  • a benzoxazine resin with a bisphenol A/aniline bicyclic structure ie, bisphenol A/aniline benzoxazine resin
  • the green environmental protection dipping liquid of the present invention is expressed in weight percentage, and its raw material composition is: 50kg of blocked isocyanate, 15kg of benzoxazine resin, 300kg of EPDM rubber, and auxiliary a (fatty alcohol polyoxyethylene ether) ) 15kg, adjuvant b (sodium hexametaphosphate) 25kg, softened water 595kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 21%.
  • a benzoxazine resin with a bisphenol A/aniline bicyclic structure ie, bisphenol A/aniline benzoxazine resin
  • the green and environmentally friendly dipping liquid of the present invention is expressed by weight percentage, and its raw material composition is: 50kg of blocked isocyanate, 60kg of benzoxazine resin, 500kg of butyl pyridine latex, and 15kg of auxiliary a (fatty alcohol polyoxyethylene ether) , Additive b (sodium hexametaphosphate) 25kg, softened water 350kg, the total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 31%.
  • This embodiment uses a phenol/MDA bicyclic benzoxazine resin (ie, a phenol/MDA type benzoxazine resin).
  • the green and environment-friendly dipping liquid of the present invention is expressed by weight percentage, and its raw material composition is: 10kg of blocked isocyanate, 100kg of benzoxazine resin, 300kg of styrene butadiene latex, and 15kg of auxiliary a (fatty alcohol polyoxyethylene ether) , Auxiliary b (aqueous calcium stearate emulsion) 25kg, softened water 550kg, the total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 30%.
  • a benzoxazine resin with a bisphenol A/aniline bicyclic structure ie, bisphenol A/aniline benzoxazine resin
  • the green and environment-friendly dipping liquid of the present invention is expressed by weight percentage, and its raw material composition is: 150kg of blocked isocyanate, 5kg of benzoxazine resin, 100kg of butadiene latex, 15kg of adjuvant a (Tween-20), Additive b (sodium hexametaphosphate) 25kg, softened water 705kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 15.0%.
  • a benzoxazine resin with a bisphenol A/aniline bicyclic structure ie, bisphenol A/aniline benzoxazine resin
  • the green environmental protection dipping liquid of the present invention is expressed in weight percentage, and its raw material composition is: 100kg of blocked isocyanate, 15kg of benzoxazine resin, 300kg of butadiene latex, 15kg of adjuvant a (Tween-80), Additive b (sodium hexametaphosphate) 25kg, softened water 545kg, the total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 24%.
  • This embodiment uses a phenol/MDA bicyclic benzoxazine resin (ie, a phenol/MDA type benzoxazine resin).
  • the green environmental protection dipping liquid of the present invention is expressed in weight percentage. Its raw material composition is: 50kg of blocked isocyanate, 15kg of benzoxazine resin, 300kg of butadiene pyridine latex, and auxiliary a (sodium diisobutyl naphthalene sulfonate) ) 15kg, additive b (aqueous calcium stearate emulsion) 25kg, softened water 595kg, total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 18.0%.
  • This embodiment uses a bisphenol F/MDA bicyclic benzoxazine resin (ie, bisphenol F/aniline benzoxazine resin).
  • the green and environmentally friendly dipping liquid of the present invention is expressed by weight percentage, and its raw material composition is: 50kg of blocked isocyanate, 60kg of benzoxazine resin, 500kg of nitrile latex, 15kg of auxiliary a (Tween-20), auxiliary Agent b (sodium hexametaphosphate) 25kg, softened water 350kg, the total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 35%.
  • This embodiment uses a bisphenol F/MDA bicyclic benzoxazine resin (ie, bisphenol F/aniline benzoxazine resin).
  • the green and environment-friendly dipping liquid of the present invention is expressed in weight percentage, and its raw material composition is: 10kg of blocked isocyanate, 100kg of benzoxazine resin, 300kg of carboxyl styrene butadiene latex, 15kg of auxiliary a (Tween-80), Additive b (sodium hexametaphosphate) 25kg, softened water 550kg, the total weight of various components is 1000kg; the solid content of the obtained dipping liquid is 30%.
  • a benzoxazine resin with a bisphenol A/aniline bicyclic structure ie, bisphenol A/aniline benzoxazine resin
  • composition 1 b. Add the weighed blocked isocyanate and auxiliary agent a into demineralized water and stir evenly to obtain composition 1;
  • the one-bath method is used for dipping.
  • the fiber skeleton material used is polyester and is exactly the same as in Examples 1-5 of the present invention, and the dipping liquid is the RFL system;
  • the existing product In 2 the fiber skeleton material used is nylon 66 and is exactly the same as in Examples 6-10 of the present invention, the dipping liquid is an RFL system;
  • the fiber skeleton material used is nylon 6 It is exactly the same as in Examples 11-15 of the present invention ,
  • the dipping liquid is RFL system.
  • Example sample test method description Test the cords after dipping in Examples 1-15 of the present invention and existing products 1-3.
  • the middle peak value of the peeling force is the adhesive peel strength; the tensile performance is in accordance with the GB/T32108-2015 method, and the dipping
  • the cord is fixed on the CRE tensile machine, and the tension is applied at a constant speed until it breaks; the dry heat shrinkage is in accordance with the GB/T30312-2013 method, and the shrinkage of the rubber cord fabric is measured after a certain period of time under hot air at a constant temperature.
  • Table 1 shows the ratio and test results of the dipping solution of the products of Examples 1-5 of the present invention and the existing product 1.
  • the embodiment of the present invention provides a green and environmentally friendly dipping liquid and its production method.
  • the green and environmentally friendly dipping liquid provided by the present invention is expressed as a percentage by weight.
  • the raw material composition is blocked isocyanate 1-15%, and special amino
  • the resin is 0.5-10%
  • the rubber latex is 10-50%
  • the auxiliary agent is 1-50%
  • the rest is water
  • the total weight percentage of each component is 100%.
  • the dipping liquid of the invention does not contain toxic and harmful substances such as formaldehyde and resorcinol, and the production method is simple and easy to operate, the production cycle is short, and the safety factor is high, and the preparation of the dipping liquid and the safe and green production of the dipping process are realized.

Abstract

一种绿色环保型浸胶液，其原料组成为封闭型异氰酸酯1～15％，特种氨基树脂0.5～10％，橡胶胶乳10～50％，助剂1～5％，其余为水，各成分重量百分含量之和为100％。所述浸胶液的制备方法为：将封闭型异氰酸酯和助剂a加入水中搅匀，得到组合物1；将助剂b加入组合物1中搅匀，得到组合物2；将特种氨基树脂加入组合物2中搅匀，然后进行研磨，得到组合物3；将橡胶胶乳加入组合物3中搅匀，得到绿色环保型浸胶液，包装。所述浸胶液不含甲醛及间苯二酚等有毒有害物质，其生产方法简单易操作，生产周期短、安全系数高，实现了浸胶液制备及浸胶过程的安全绿色生产。

Description

一种绿色环保型浸胶液及其生产方法
交叉引用
本发明要求在中国专利局提交的、申请号为201910607037.3、发明名称为“一种绿色环保型浸胶液及其生产方法”的中国专利申请的优先权，该申请的全部内容通过引用结合在本发明中。
技术领域
本发明涉及浸胶制备技术领域，具体涉及一种不含甲醛及间苯二酚、环境友好型的绿色环保型浸胶液及其生产方法。
背景技术
近年来，随着汽车制造业和交通运输业(尤其是高速公路)的迅猛发展，性能优越的子午线轮胎需求增长迅速。子午线轮胎的骨架材料多是采用锦纶、涤纶、芳纶等纤维织品，需要橡胶与锦纶等纤维织品之间有效的粘合。为了提高纤维与橡胶材料之间的粘合作用，人们通过研究在1935年发明了间苯二酚-甲醛-胶乳(RLF)粘合体系，并一直沿用至今。被时间证明对于橡胶与纤维粘合是最有效、经济的粘合体系。
随着经济高速发展，人们对橡胶制品、橡胶骨架材料的需求日益增加。同时环境保护意识、职业健康安全意识的觉醒，使人们对间苯二酚、甲醛等化学品的关注越来越多。世界各国开始从法律法规、行业规范等方面纷纷向减少、甚至杜绝使用有害化学品方向发展。
国家工信部等部委发布的《国家鼓励的有毒有害原料(产品)替代品目录(2016)》中：二、有机污染物替代的第6、7项，将“酚醛树脂(RLF)浸渍剂”列入被替代品。随着欧盟轮胎标签法及世界各地关于绿色轮胎相关法律法规的实施，轮胎原料绿色化进程得以迅速推进。目前橡胶和橡胶骨架材料的粘合体系多采用RFL(间苯二酚、甲醛、胶乳)，其中间苯二酚和甲醛的含量已明确限制。同时RFL体系中间苯二酚、氨水等原料具有恶臭和刺激性气味，配制车间易产生异味；而甲醛溶液又作为危险化学品，在储存和使用过程中有较高的安全管理要求，提升了浸胶液配制车间的防爆等级。
在各种文献资料和专利中已经报道了用于提高有机纤维材料浸胶后粘 合力等应用性能指标的不含甲醛及间苯二酚的浸胶液。
固特异公司目前采用的一种浸渍剂主要由一种或两种丙稀酸类单体与少量苯乙烯共聚制得丙烯酸树脂，用此丙烯酸树脂混合胶乳制得浸胶配方。用于非活化类聚酯纤维时，需要经过一浴环氧化合物等活化，二浴丙烯酸树脂-胶乳体系浸胶两步完成，骨架材料浸胶后性能与应用传统的RFL体系浸胶后接近，但整体工艺流程复杂，设备投入较高，且原材料都是其指定供应商，对上游产品的依赖程度较高。
倍耐力轮胎有限公司目前的专利保护配方至少包含橡胶胶乳、环氧化合物和分子量大于190道尔顿的多胺。在结构原件中，这些组合物在骨架材料和胶料之间产生的粘性和该行业中使用的传统RFL体系的粘性接近。但是配方中使用的多胺原材料要求苛刻，采购成本较高，且在传统生产车间使用多胺类原材料与当下的环保政策不符，在浸胶流程中容易出现粘毂导致阶段性停产检修等不利于连续生产等不利因素。
公开于该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解，而不应当被视为承认或以任何形式暗示该信息构成已为本领域一般技术人员所公知的现有技术。
发明内容
本发明要解决的技术问题是：针对上述浸胶液存在的技术问题，本发明提供一种绿色环保型浸胶液及其生产方法。本发明浸胶液不含甲醛及间苯二酚等有毒有害物质，其生产方法简单易操作，生产周期短、安全系数高，实现了的浸胶液制备及浸胶过程的安全绿色生产。
为了解决上述问题，本发明采取的技术方案是：
本发明提供一种绿色环保型浸胶液，以重量百分含量表示，所述绿色环保型浸胶液的原料组成为：封闭型异氰酸酯1～15％，特种氨基树脂0.5～10％，橡胶胶乳10～50％，助剂1～5％，其余为水，各成分重量百分含量之和为100％；
所述助剂由助剂a和助剂b组成，二者之间的质量配比为1：1～3。
根据上述的绿色环保型浸胶液，以重量百分含量表示，所述绿色环保型浸胶液的原料组成为：封闭型异氰酸酯1～5％，特种氨基树脂1.5～10％，橡胶胶乳20～40％，助剂3～5％，其余为水，各成分重量百分含量之和为100％；
所述助剂由助剂a和助剂b组成，二者之间的质量配比为1：1～3。
根据上述的绿色环保型浸胶液，所述特种氨基树脂为脲醛树脂、三聚氰胺甲醛树脂、苯并噁嗪树脂和聚酰胺多胺环氧氯丙烷中的一种或多种。
根据上述的绿色环保型浸胶液，所述橡胶胶乳为丁吡胶乳、丁二烯胶乳、三元乙丙橡胶、丁苯胶乳、天然胶乳、丁腈胶乳、羧基丁吡胶乳、羧基丁苯胶乳和羧基丁腈胶乳中的一种或多种。
根据上述的绿色环保型浸胶液，所述助剂a为吐温-20、二异丁基萘磺酸钠、吐温80或脂肪醇聚氧乙烯醚。
根据上述的绿色环保型浸胶液，所述助剂b为高粒度高岭土瓷土湿法超细研磨助剂、水性硬脂酸钙乳液或六偏磷酸钠。
根据上述的绿色环保型浸胶液，所述浸胶液的固含量为5～30％。
另外，提供一种绿色环保型浸胶液的生产方法，所述生产方法包括以下步骤：
a、首先按照上述绿色环保型浸胶液的配比比例称取各种原料；
b、将称取的封闭型异氰酸酯和助剂a加入水中并搅拌均匀，得到组合物1；
c、然后将助剂b加入所得组合物1中并搅拌均匀，得到组合物2；
d、接着将特种氨基树脂加入所得组合物2中并搅拌均匀，然后进行研磨，得到组合物3；
e、将橡胶胶乳加入所得组合物3中并搅拌均匀，得到绿色环保型浸胶液，包装。
根据上述的绿色环保型浸胶液的生产方法，步骤d中所述研磨后组合物3中固体粒度分布为1～50μm。
有益效果
1、本发明浸胶液是通过在有机纤维材料和橡胶之间提供一种或多种作用力使得有机纤维材料和橡胶相互粘合而成；本发明浸胶液以封闭性异氰酸酯、特种氨基树脂等为主要成分，不含甲醛及间苯二酚等有毒有害物质；其生产方法简单易操作，生产周期短、安全系数高。从而实现了浸胶液制备及浸胶过程的安全绿色生产，而且整个生产过程中不存在废弃物质的产生，环境友好。
2、本发明浸胶液，与原有的RFL浸胶液现配现用不同，该浸胶液可以稳定储存及运输，填补了目前商品市场的空白。
附图说明
一个或多个实施例通过与之对应的附图中的图片进行示例性说明，这些示例性说明并不构成对实施例的限定。在这里专用的词“示例性”意为“用作例子、实施例或说明性”。这里作为“示例性”所说明的任何实施例不必解释为优于或好于其它实施例。
图1为本发明绿色环保型浸胶液制备方法的工艺流程示意图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合一个或多个实施例以及与之对应的附图对本发明实施例中的技术方案进行清楚、完整的示例性说明。
显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。除非另有其它明确表示，否则在整个说明书和权利要求书中，术语“包括”或其变换如“包含”或“包括有”等等将被理解为包括所陈述的组成部分，而并未排除其它元件或其它组成部分。
这些实施例并不构成对保护范围的限定。除非另有说明，这里的任何实施例不必解释为优于或好于其它实施例。
另外，为了更好的说明本发明，在下文的实施例中给出了众多的具体细节。本领域技术人员应当理解，没有某些具体细节，本发明同样可以实施。在一些实施例中，对于本领域技术人员熟知的方法、手段、元件、通常按照常规条件以及手册中所述的条件或按照制造厂商所建议的条件的实验方法未作详细描述，以便于凸显本发明的主旨。所用的材料、试剂等，如无特殊说明，均为常规可由商业途径获得的。
以下实施例中，所用的原料均为市售商品，其中：
封闭型异氰酸酯，其粘度：200-500mpa.s/25℃，固含50±1.5％，密度：1.0±0.2g/cm 3(20℃)，粒度，≤5μm；
双酚A/苯胺型苯并噁嗪树脂，MW为466-800，软化点50-90℃，凝胶时间(210℃，1g)100-400秒；
苯酚/MDA型苯并噁嗪树脂，MW为438-800，软化点50-90℃，凝胶 时间(210℃，1g)100-400秒；
双酚F/苯胺型苯并噁嗪树脂，MW为438-800，软化点50-90℃，凝胶时间(210℃，1g)100-400秒；
丁吡胶乳，粘度为20-45mpa.s/25℃，固含39.5-41.5％，密度：0.980-0.990g/cm 3(20℃)，pH为10-12；
羧基丁苯胶乳，粘度为4-350mpa.s/25℃，固含48.0-54.0％，密度：0.970-0.100g/cm 3(20℃)，pH为7.0-9.0；
丁苯胶乳，粘度为200-800mpa.s/25℃，固含48.0-61.0％，密度：0.960-0.980g/cm 3(20℃)，pH为8.0-10.5；
丁二烯胶乳，粘度为10-50mpa.s/25℃，固含48.0-54.0％，密度：1.01-1.20g/cm 3(20℃)，pH为12.0-14.0；
丁腈胶乳，其粘度为7-50mpa.s/25℃，固含43.0-45.0％，pH为7.0-8.0；
羧基丁苯胶乳，其粘度为4-350mpa.s/25℃，固含48.0-54.0％，密度：0.970-0.100g/cm 3(20℃)，pH为7.0-9.0。
实施例1
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯150kg，苯并噁嗪树脂5kg，丁吡胶乳100kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水705kg，各种成分总重量为1000kg；所得浸胶液的固含量为15.0％。
本实施例采用的是双酚A/苯胺双环结构的苯并噁嗪树脂(即双酚A/苯胺型苯并噁嗪树脂)。
实施例2
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯100kg，苯并噁嗪树脂15kg，羧基丁苯胶乳300kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水545kg，各种成分总重量为1000kg；所得浸胶液的固含量为24％。
本实施例采用的是苯酚/MDA双环结构的苯并噁嗪树脂(即苯酚/MDA型苯并噁嗪树脂)。
实施例3
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯50kg，苯并噁嗪树脂15kg，丁吡胶乳300kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水595kg，各种成 分总重量为1000kg；所得浸胶液的固含量为18.0％。
本实施例采用的是双酚F/MDA双环结构的苯并噁嗪树脂(即双酚F/苯胺型苯并噁嗪树脂)。
实施例4
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯50kg，苯并噁嗪树脂60kg，羧基丁苯胶乳500kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水350kg，各种成分总重量为1000kg；所得浸胶液的固含量为35.5％。
本实施例采用的是双酚F/MDA双环结构的苯并噁嗪树脂(即双酚F/苯胺型苯并噁嗪树脂)。
实施例5
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯10kg，苯并噁嗪树脂100kg，羧基丁苯胶乳300kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水550kg，各种成分总重量为1000kg；所得浸胶液的固含量为30％。
本实施例采用的是双酚A/苯胺双环结构的苯并噁嗪树脂(即双酚A/苯胺型苯并噁嗪树脂)。
实施例6
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯150kg，苯并噁嗪树脂5kg，三元乙丙橡胶100kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水705kg，各种成分总重量为1000kg；所得浸胶液的固含量为15.0％。
本实施例采用的是双酚A/苯胺双环结构的苯并噁嗪树脂(即双酚A/苯胺型苯并噁嗪树脂)。
实施例7
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯100kg，苯并噁嗪树脂15kg，三元乙丙橡胶300kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水545kg，各种成分总重量为1000kg；所得浸胶液的固含量为24％。
本实施例采用的是双酚A/苯胺双环结构的苯并噁嗪树脂(即双酚A/苯胺型苯并噁嗪树脂)。
实施例8
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯50kg，苯并噁嗪树脂15kg，三元乙丙橡胶300kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水595kg，各种成分总重量为1000kg；所得浸胶液的固含量为21％。
本实施例采用的是双酚A/苯胺双环结构的苯并噁嗪树脂(即双酚A/苯胺型苯并噁嗪树脂)。
实施例9
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯50kg，苯并噁嗪树脂60kg，丁吡胶乳500kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(六偏磷酸钠)25kg，软化水350kg，各种成分总重量为1000kg；所得浸胶液的固含量为31％。
本实施例采用的是苯酚/MDA双环结构的苯并噁嗪树脂(即苯酚/MDA型苯并噁嗪树脂)。
实施例10
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯10kg，苯并噁嗪树脂100kg，丁苯胶乳300kg，助剂a(脂肪醇聚氧乙烯醚)15kg，助剂b(水性硬脂酸钙乳液)25kg，软化水550kg，各种成分总重量为1000kg；所得浸胶液的固含量为30％。
本实施例采用的是双酚A/苯胺双环结构的苯并噁嗪树脂(即双酚A/苯胺型苯并噁嗪树脂)。
实施例11
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯150kg，苯并噁嗪树脂5kg，丁二烯胶乳100kg，助剂a(吐温-20)15kg，助剂b(六偏磷酸钠)25kg，软化水705kg，各种成分总重量为1000kg；所得浸胶液的固含量为15.0％。
本实施例采用的是双酚A/苯胺双环结构的苯并噁嗪树脂(即双酚A/苯胺型苯并噁嗪树脂)。
实施例12
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯100kg，苯并噁嗪树脂15kg，丁二烯胶乳300kg，助剂a(吐温-80)15kg，助剂b(六偏磷酸钠)25kg，软化水545kg，各种成分总重量为1000kg；所得浸胶液的固含量为24％。
本实施例采用的是苯酚/MDA双环结构的苯并噁嗪树脂(即苯酚/MDA型苯并噁嗪树脂)。
实施例13
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯50kg，苯并噁嗪树脂15kg，丁吡胶乳300kg，助剂a(二异丁基萘磺酸钠)15kg，助剂b(水性硬脂酸钙乳液)25kg，软化水595kg，各种成分总重量为1000kg；所得浸胶液的固含量为18.0％。
本实施例采用的是双酚F/MDA双环结构的苯并噁嗪树脂(即双酚F/苯胺型苯并噁嗪树脂)。
实施例14
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯50kg，苯并噁嗪树脂60kg，丁腈胶乳500kg，助剂a(吐温-20)15kg，助剂b(六偏磷酸钠)25kg，软化水350kg，各种成分总重量为1000kg；所得浸胶液的固含量为35％。
本实施例采用的是双酚F/MDA双环结构的苯并噁嗪树脂(即双酚F/苯胺型苯并噁嗪树脂)。
实施例15
本发明绿色环保型浸胶液，以重量百分含量表示，其原料组成为：封闭型异氰酸酯10kg，苯并噁嗪树脂100kg，羧基丁苯胶乳300kg，助剂a(吐温-80)15kg，助剂b(六偏磷酸钠)25kg，软化水550kg，各种成分总重量为1000kg；所得浸胶液的固含量为30％。
本实施例采用的是双酚A/苯胺双环结构的苯并噁嗪树脂(即双酚A/苯胺型苯并噁嗪树脂)。
本发明实施例1-15绿色环保型浸胶液的制备方法：
a、首先按照实施例1-15任一所述绿色环保型浸胶液的配比比例称取各种原料；
b、将称取的封闭型异氰酸酯和助剂a加入软化水中并搅拌均匀，得到组合物1；
c、然后将助剂b加入所得组合物1中并搅拌均匀，得到组合物2；
d、接着将特种氨基树脂加入所得组合物2中并搅拌均匀，然后进行研磨，直至固体粒度小于5μm，得到组合物3；
e、将橡胶胶乳加入所得组合物3中并搅拌均匀，得到绿色环保型浸胶 液，包装。
本发明实施例1-15所得产品绿色环保型浸胶液和现有传统产品的相关性能对比如下：
实施例中浸胶方法及材料说明：本发明实施例1-15中均采用一浴法浸胶。为保证实验数据的一致可对比性，作为对照样品，现有产品1中，采用的纤维骨架材料为涤纶并与本发明实施例1-5中完全相同，浸胶液为RFL体系；现有产品2中，采用的纤维骨架材料为锦纶66并与本发明实施例6-10中完全相同，浸胶液为RFL体系；采用的纤维骨架材料为锦纶6与本发明实施例11-15中完全相同，浸胶液为RFL体系。
实施例样品测试方法说明：对本发明实施例1-15和现有产品1-3浸胶处理后的帘线进行测试，测试方法：附胶量按照GB/T30310-2013方法，使用指定溶剂溶解浸胶帘子布，测定剩余固体量；H粘合力按照GB/T2942-2009方法，测量单根帘线从硫化橡胶块中抽出所需要的力；剥离表面粘合力按照GB/T32109-2015方法，使用垃圾试验机恒速剥离浸胶帘子布和橡胶制成的式样模坯，剥离力的中峰值即为粘合剥离强度；拉伸性能按照GB/T32108-2015方法，在规定条件下，将浸胶线绳固定在CRE型拉力机上，恒速施加拉力，直至断裂；干热收缩率按照GB/T30312-2013方法，在恒定温度的热空气下，一定时间后测定进胶帘子布的收缩情况。
本发明实施例1-5产品和现有产品1的浸胶液配比及测试结果见表1。
表1实施例1-5和现有产品1的浸胶液配比及测试结果
Figure PCTCN2020099960-appb-000001
Figure PCTCN2020099960-appb-000002
本发明实施例6-10和现有产品2的浸胶液配比及测试结果详见表2。
表2本发明实施例6-10和现有产品2的浸胶液配比及测试结果
Figure PCTCN2020099960-appb-000003
Figure PCTCN2020099960-appb-000004
本发明实施例11-15和现有产品3的浸胶液配比及测试结果详见表3。
表3本发明实施例11-15和现有产品3的浸胶液配比及测试结果
Figure PCTCN2020099960-appb-000005
Figure PCTCN2020099960-appb-000006
表1-3中结果说明本发明的浸胶液在不含间苯二酚、甲醛等组分情况下，涤纶帘线和橡胶可以有良好的粘合效果，达到了传统RFL相同的粘合水平，完全可以替代RFL浸胶液。
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
工业实用性
本发明实施例提供的一种绿色环保型浸胶液及其生产方法，本发明提供的绿色环保型浸胶液，以重量百分含量表示，原料组成为封闭型异氰酸酯1～15％，特种氨基树脂0.5～10％，橡胶胶乳10～50％，助剂1～5％，其余为水，各成分重量百分含量之和为100％。本发明浸胶液不含甲醛及间苯二酚等有毒有害物质，其生产方法简单易操作，生产周期短、安全系数高，实现了的浸胶液制备及浸胶过程的安全绿色生产。

Claims (9)

  1. 一种绿色环保型浸胶液，其特征在于，以重量百分含量表示，所述绿色环保型浸胶液的原料组成为：封闭型异氰酸酯1～15％，特种氨基树脂0.5～10％，橡胶胶乳10～50％，助剂1～5％，其余为水，各成分重量百分含量之和为100％；
    所述助剂由助剂a和助剂b组成，二者之间的质量配比为1：1～3。
  2. 根据权利要求1所述的绿色环保型浸胶液，其特征在于：以重量百分含量表示，所述绿色环保型浸胶液的原料组成为：封闭型异氰酸酯1～5％，特种氨基树脂1.5～10％，橡胶胶乳20～40％，助剂3～5％，其余为水，各成分重量百分含量之和为100％；
    所述助剂由助剂a和助剂b组成，二者之间的质量配比为1：1～3。
  3. 根据权利要求1所述的绿色环保型浸胶液，其特征在于：所述特种氨基树脂为脲醛树脂、三聚氰胺甲醛树脂、苯并噁嗪树脂和聚酰胺多胺环氧氯丙烷中的一种或多种。
  4. 根据权利要求1所述的绿色环保型浸胶液，其特征在于：所述橡胶胶乳为丁吡胶乳、丁二烯胶乳、三元乙丙橡胶、丁苯胶乳、天然胶乳、丁腈胶乳、羧基丁吡胶乳、羧基丁苯胶乳和羧基丁腈胶乳中的一种或多种。
  5. 根据权利要求1所述的绿色环保型浸胶液，其特征在于：所述助剂a为吐温-20、二异丁基萘磺酸钠、吐温-80或脂肪醇聚氧乙烯醚。
  6. 根据权利要求1所述的绿色环保型浸胶液，其特征在于：所述助剂b为高粒度高岭土瓷土湿法超细研磨助剂、水性硬脂酸钙乳液或六偏磷酸钠。
  7. 根据权利要求1所述的绿色环保型浸胶液，其特征在于：所述绿色环保型浸胶液的固含量为5～30％。
  8. 一种绿色环保型浸胶液的生产方法，其特征在于，所述生产方法包括以下步骤：
    a、首先按照上述绿色环保型浸胶液的配比比例称取各种原料；
    b、将称取的封闭型异氰酸酯和助剂a加入水中并搅拌均匀，得到组合物1；
    c、然后将助剂b加入所得组合物1中并搅拌均匀，得到组合物2；
    d、接着将特种氨基树脂加入所得组合物2中并搅拌均匀，然后进行研磨， 得到组合物3；
    e、将橡胶胶乳加入所得组合物3中并搅拌均匀，得到绿色环保型浸胶液，包装。
  9. 根据权利要求8所述的绿色环保型浸胶液的生产方法，其特征在于：步骤d中所述研磨后组合物3中固体粒度分布为1～50μm。
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