CN102587144A - Preparation method for aramid fiber-organic silicon composite material - Google Patents
Preparation method for aramid fiber-organic silicon composite material Download PDFInfo
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- CN102587144A CN102587144A CN2012100378779A CN201210037877A CN102587144A CN 102587144 A CN102587144 A CN 102587144A CN 2012100378779 A CN2012100378779 A CN 2012100378779A CN 201210037877 A CN201210037877 A CN 201210037877A CN 102587144 A CN102587144 A CN 102587144A
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Abstract
The invention relates to a preparation method for an aramid fiber-organic silicon composite material. The preparation method comprises the following steps of: (1) blending organic silicon modified polyurethane, a reinforcing agent and a cross-linking agent, and applying the mixed organic silicon modified polyurethane, reinforcing agent and cross-linking agent to the surface of an aramid fiber textile by using steeping, roller coating and knife coating technologies, and backing for 1-10 minutes at the temperature of 100-150 DEG C; (2) uniformly coating a liquid silicon rubber on the surface of the aramid fiber textile once or more than once by using a scraping knife or a rotary drum, and vulcanizing at the temperature of 100-150 DEG C to prepare the aramid fiber-organic silicon composite material. According to the preparation method, the blocking type organic silicon modified polyurethane is used for preparing the aramid fiber-organic silicon composite material so that the peel strength between the aramid fiber textile and the organic silicon is enhanced; the technology is simple and easy to implement; and the prepared aramid fiber-organic silicon composite material has the characteristics of high tensile strength, low temperature resistance, high temperature resistance, ageing resistance, flame retardance and the like and can be used for awning cloth, wind shields of trains and conveyor belts.
Description
Technical field
The present invention relates to the preparation method of a kind of aramid fiber-organosilicon composite.
Background technology
Aramid fiber-organic silicon coating composite is composited by aryl fiber cloth and elastomer silicone; It is one type of high performance environmentally friendly product; In conjunction with the plurality of advantages of aramid fiber and elastomer silicone; With respect to the present coating composite material of widely used other fibers (like nylon, terylene etc.) and other elastomers (like natural rubber, EP rubbers, acrylic acid ester, polyurethane, polyvinyl chloride, sulfonation vinyl chloride etc.), have higher intensity, more excellent flame, weatherability, high-low temperature resistant and chemicals-resistant corrosive nature.And the characteristics of organosilicon macromolecule make 100% organic silicon coating adhesive have good mobility, in preparation organic silicon coating composite material, do not need with an organic solvent or on a small quantity with an organic solvent, have reduced environmental pollution and energy consumption.
In view of the high strength of aramid fiber-organic silicon coating composite, excellent high flame resistance, aramid fiber-organic silicon coating composite has been applied to the windscreen material of the corrugated hinge section in compartment of bullet train, subway train abroad, conveyor materials.
The aramid fiber macromolecular chain has very high rigidity, and has highly crystalline between strand, and the surface of aramid fiber has suitable inertia, causes aramid fiber and other materials binding ability poor, particularly and the adhesion between elastomer silicone more undesirable.In order to improve the adhesion between aramid fiber and elastomer silicone, carried out number of research projects both at home and abroad, mainly comprise: modification is carried out to aramid fiber surface in (1), improves the activity of aramid fiber surface; (2) select the suitable aramid fiber structure of weaving cotton cloth, increase that aramid fiber is weaved cotton cloth and elastomer silicone between contact area, the chemical composition of (3) liquid towards organic silica gel is adjusted, and in liquid organosilicon glue, adds active higher crosslinking agent and binder component.The method of at present aramid fiber surface being handled comprises surface etching treatment, surface graft modification, plasma treatment, gamma-rays radiation and sonicated etc.; But these processing methods can't be handled by mass because of being difficult to control usually; And possibly damage aramid fiber intensity, therefore in commercial production, use less.
The liquid towards organic silica gel carries out the component adjustment, in the process of preparation liquid organosilicon glue, adds different crosslinked or adhesives, also can improve the adhesion between elastomer silicone and fabric.This method does not influence production efficiency; Can not reduce the intensity of fabric yet; In the process of obtaining liq organic silica gel, can also add other functional aid, like fire retardant, functional tiny balloon etc.; Having made final coated fabric goods have more excellent properties and function, is to prepare the research important directions that aramid fiber strengthens elastomer silicone at present.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of aramid fiber-organosilicon composite, can obviously improve the peel strength between aramid fiber and organosilicon polymer.
In order to achieve the above object, the technical scheme of the present invention's employing is:
The preparation method of a kind of aramid fiber-organosilicon composite may further comprise the steps:
(1) organic silicon modified polyurethane, reinforcing agent and crosslinking agent are mixed; Through dipping, roller coating and blade coating technology mixed organic silicon modified polyurethane, reinforcing agent and crosslinking agent are applied to the kevlar fabric surface, and training was dried by the fire 1～10 minute under 100～150 ℃ of conditions;
(2) use scraper or cylinder one or many that liquid silastic is evenly coated said kevlar fabric surface, after 100～150 ℃ of sulfurations, make aramid fiber-organosilicon composite.
In the such scheme, the synthetic method of said organic silicon modified polyurethane comprises the steps:
Steps A makes end containing hydrogen silicone oil and vinyl polyethers that graft reaction take place under the effect of catalyst, obtains first intermediate;
Step B obtains second intermediate with said first intermediate and isocyanate reaction;
Step C reacts said second intermediate and end-capping reagent, obtains the end-sealed type organic silicon modified polyurethane.
In the such scheme; Graft reaction takes place in said steps A middle-end containing hydrogen silicone oil and vinyl polyethers under the effect of catalyst; Specifically comprise: said end containing hydrogen silicone oil and said vinyl polyethers are joined in the reactor by 1: 1.8～2.4 mol ratio, be warming up to 60～100 ℃ after stirring, add catalyst again; React after 2～6 hours, obtain first intermediate.
In the such scheme; Among the said step B said first intermediate and isocyanate reaction are obtained second intermediate; Specifically comprise: said first intermediate is warming up to 50～80 ℃; Added said isocyanate reaction 2～6 hours, the molar weight of said isocyanates is 1.1～1.4 times of said end containing hydrogen silicone oil, and reaction obtains said second intermediate after accomplishing.
In the such scheme; Among the said step C said second intermediate and end-capping reagent are reacted; Specifically comprise: said second intermediate is warming up to 50～80 ℃, drips said end-capping reagent reaction 2～6 hours, the molar weight of said end-capping reagent is 0.1～0.4 times of said end containing hydrogen silicone oil.
In the such scheme, the end containing hydrogen silicone oil in the said steps A comprises the hydrogeneous methyl-silicone oil of end, holds hydrogeneous ethyl silicon oil, end one or more in hydrogeneous phenyl silicone oil.
In the such scheme, the structure of vinyl polyethers is CH in the said steps A
2=CH-(CH
2CH
2O) n-OH or CH
2=C (CH
3)-(CH
2CH
2O) n-OH.
In the such scheme, the catalyst in the said steps A is chloroplatinic acid catalyst or cassette (Karstedt) platinum catalyst.
In the such scheme; Isocyanates among the said step B is toluene di-isocyanate(TDI) (TDI); Methyl diphenylene diisocyanate (MDI); IPDI (IPDI), dicyclohexyl methyl hydride diisocyanate (HMDI), one or more in the polymer of hexamethylene diisocyanate (HDI) and said isocyanates.
In the such scheme, the end-capping reagent among the said step C comprises a kind of in cyclohexanone oxime, methyl ethyl ketoxime, ethyl acetoacetate, sodium hydrogensulfite, caprolactam, the beta-propiolactone.
In the such scheme, said reinforcing agent is one or more in white carbon, calcium carbonate, the zinc oxide.
In the such scheme, said crosslinking agent is polyalcohol or polyamine compounds.
Compare with the prior art scheme, the beneficial effect that the technical scheme that the present invention adopts produces is following:
The present invention is used to prepare aramid fiber-organosilicon composite with the end-sealed type organic silicon modified polyurethane, has strengthened the peel strength between kevlar fabric and organosilicon, and technology is simply easy to implement; Prepared aramid fiber-organosilicon composite has high-tensile strength, characteristic such as low temperature resistant, high temperature resistant, ageing-resistant, fire-retardant, can be used for tarpaulin, train windscreen, conveyer belt.
The specific embodiment
Below in conjunction with embodiment technical scheme of the present invention is described in detail.
Present embodiment provides the preparation method of a kind of aramid fiber-organosilicon composite, may further comprise the steps:
(1) organic silicon modified polyurethane, reinforcing agent and crosslinking agent are mixed; Through dipping, roller coating and blade coating technology mixed organic silicon modified polyurethane, reinforcing agent and crosslinking agent are applied to the kevlar fabric surface; And training was dried by the fire 1～10 minute under 100～150 ℃ of conditions, and preferably training was dried by the fire 3 minutes under 110 ℃ of conditions;
(2) use scraper or cylinder one or many that liquid silica gel is evenly coated the kevlar fabric surface, make aramid fiber-organosilicon composite after 5 minutes, preferably through 130 ℃ of sulfurations through 100～150 ℃ of sulfurations.
In the present embodiment, reinforcing agent is one or more in white carbon, calcium carbonate, the zinc oxide.
In the present embodiment, crosslinking agent is polyalcohol or polyamine compounds.
In the present embodiment, the synthetic method of organic silicon modified polyurethane specifically comprises the steps:
Steps A, graft reaction takes place in end containing hydrogen silicone oil and vinyl polyethers under the effect of catalyst, specifically comprise: will hold containing hydrogen silicone oil and vinyl polyethers to join in the reactor by 1: 1.8～2.4 mol ratio; Preferably mol ratio is 1: 2; Be warming up to 60～100 ℃ after stirring, preferably be warming up to 90 ℃, add catalyst again; React after 2～6 hours, obtain first intermediate; Wherein, the end containing hydrogen silicone oil comprise the hydrogeneous methyl-silicone oil of end, hold hydrogeneous ethyl silicon oil, end one or more in hydrogeneous phenyl silicone oil; The structure of vinyl polyethers is CH
2=CH-(CH
2CH
2O) n-OH or CH
2=C (CH
3)-(CH
2CH
2O) n-OH; Catalyst is chloroplatinic acid catalyst or cassette (Karstedt) platinum catalyst;
Step B obtains second intermediate with first intermediate and isocyanate reaction, specifically comprises: first intermediate is warming up to 50～80 ℃; Preferably be warming up to 70 ℃; Added isocyanate reaction 2～6 hours, preferably reacted 4 hours, reaction obtains second intermediate after accomplishing; The molar weight of isocyanates is preferably 1.2 times for 1.1～1.4 times of the end containing hydrogen silicone oil; Isocyanates is toluene di-isocyanate(TDI) (TDI); Methyl diphenylene diisocyanate (MDI); IPDI (IPDI), dicyclohexyl methyl hydride diisocyanate (HMDI), one or more in the polymer of hexamethylene diisocyanate (HDI) and said isocyanates; The polymer of isocyanates can be TDI, and its polymer has the TDI dimer, TDI tripolymer etc.;
Step C; Second intermediate and end-capping reagent are reacted, specifically comprise: second intermediate is warming up to 50～80 ℃, preferably is warming up to 70 ℃; Drip end-capping reagent reaction 2～6 hours; Preferably reacted 4 hours, the molar weight of end-capping reagent is preferably 0.2 times for 0.1～0.4 times of the end containing hydrogen silicone oil; End-capping reagent comprises a kind of in cyclohexanone oxime, methyl ethyl ketoxime, ethyl acetoacetate, sodium hydrogensulfite, caprolactam, the beta-propiolactone.
The end-sealed type organic silicon modified polyurethane that is synthesized in the embodiment of the invention; At room temperature has good stable property; Can be coated on kevlar fabric easily, and activation at a certain temperature, under the effect of crosslinking agent; Form grafting and cross-linked structure with the kevlar fabric surface, can obviously improve the peel strength between kevlar fabric and organic silicon coating.The end-sealed type organic silicon modified polyurethane that is synthesized also can directly add in the liquid organosilicon glue, uses as stripping enhancing agent, to improve the tack between organic silicon coating and kevlar fabric.
Technology of the present invention is simply easy to implement, and prepared aramid fiber-organosilicon composite has high-tensile strength, characteristic such as low temperature resistant, high temperature resistant, ageing-resistant, fire-retardant, can be used for tarpaulin, train windscreen, conveyer belt.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of aramid fiber-organosilicon composite is characterized in that, may further comprise the steps:
(1) organic silicon modified polyurethane, reinforcing agent and crosslinking agent are mixed; Through dipping, roller coating and blade coating technology mixed organic silicon modified polyurethane, reinforcing agent and crosslinking agent are applied to the kevlar fabric surface, and training was dried by the fire 1～10 minute under 100～150 ℃ of conditions;
(2) use scraper or cylinder one or many that liquid silastic is evenly coated said kevlar fabric surface, after 100～150 ℃ of sulfurations, make aramid fiber-organosilicon composite.
2. the preparation method of aramid fiber as claimed in claim 1-organosilicon composite is characterized in that, synthesizing of said organic silicon modified polyurethane comprises the steps:
Steps A makes end containing hydrogen silicone oil and vinyl polyethers that graft reaction take place under the effect of catalyst, obtains first intermediate;
Step B obtains second intermediate with said first intermediate and isocyanate reaction;
Step C reacts said second intermediate and end-capping reagent, obtains the end-sealed type organic silicon modified polyurethane.
3. the preparation method of aramid fiber as claimed in claim 2-organosilicon composite; It is characterized in that graft reaction takes place for said steps A middle-end containing hydrogen silicone oil and vinyl polyethers, specifically comprises under the effect of catalyst: said end containing hydrogen silicone oil and said vinyl polyethers are joined in the reactor by 1: 1.8～2.4 mol ratio; Be warming up to 60～100 ℃ after stirring; Add catalyst again, react after 2～6 hours, obtain first intermediate.
4. the preparation method of aramid fiber as claimed in claim 2-organosilicon composite is characterized in that, the end containing hydrogen silicone oil in the said steps A comprises the hydrogeneous methyl-silicone oil of end, holds hydrogeneous ethyl silicon oil, end one or more in hydrogeneous phenyl silicone oil; The structure of vinyl polyethers is CH in the said steps A
2=CH-(CH
2CH
2O) n-OH or CH
2=C (CH
3)-(CH
2CH
2O) n-OH; Catalyst in the said steps A is chloroplatinic acid catalyst or cassette (Karstedt) platinum catalyst.
5. the preparation method of aramid fiber as claimed in claim 2-organosilicon composite; It is characterized in that; Among the said step B said first intermediate and isocyanate reaction are obtained second intermediate, specifically comprise: said first intermediate is warming up to 50～80 ℃, added said isocyanate reaction 2～6 hours; The molar weight of said isocyanates is 1.1～1.4 times of said end containing hydrogen silicone oil, and reaction obtains said second intermediate after accomplishing.
6. the preparation method of aramid fiber as claimed in claim 2-organosilicon composite; It is characterized in that; Isocyanates among the said step B is toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate (MDI), IPDI (IPDI); Dicyclohexyl methyl hydride diisocyanate (HMDI), one or more in the polymer of hexamethylene diisocyanate (HDI) and said isocyanates.
7. the preparation method of aramid fiber as claimed in claim 2-organosilicon composite; It is characterized in that; Among the said step C said second intermediate and end-capping reagent are reacted; Specifically comprise: said second intermediate is warming up to 50～80 ℃, drips said end-capping reagent reaction 2～6 hours, the molar weight of said end-capping reagent is 0.1～0.4 times of said end containing hydrogen silicone oil.
8. the preparation method of aramid fiber as claimed in claim 2-organosilicon composite is characterized in that, the end-capping reagent among the said step C comprises a kind of in cyclohexanone oxime, methyl ethyl ketoxime, ethyl acetoacetate, sodium hydrogensulfite, caprolactam, the beta-propiolactone.
9. the preparation method of aramid fiber as claimed in claim 1-organosilicon composite is characterized in that, said reinforcing agent is one or more in white carbon, calcium carbonate, the zinc oxide.
10. the preparation method of aramid fiber as claimed in claim 1-organosilicon composite is characterized in that, said crosslinking agent is polyalcohol or polyamine compounds.
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Cited By (9)
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| CN103351461A (en) * | 2013-06-26 | 2013-10-16 | 佛山市顺德区德美瓦克有机硅有限公司 | Blocked isocyanate modified polyether organic silicon and preparation method thereof |
| CN103687989A (en) * | 2012-07-19 | 2014-03-26 | 大宇国际株式会社 | Synthetic leather production method using different liquid silicone rubber coating solutions |
| CN103819901A (en) * | 2014-02-20 | 2014-05-28 | 佛山市加德纳机械配件有限公司 | Silica gel high-temperature resistant synchronous belt |
| CN104131455A (en) * | 2013-05-02 | 2014-11-05 | 黑龙江弘宇短纤维新材料股份有限公司 | Preparation method of pre-treated short aramid fiber used for rubber product |
| CN109667143A (en) * | 2018-12-19 | 2019-04-23 | 青岛天邦线业有限公司 | A kind of fiberglass threads impregnation RFL inorganic agent and preparation method thereof |
| CN110904691A (en) * | 2019-10-18 | 2020-03-24 | 安徽华烨特种材料有限公司 | Preparation process of organic silicon modified aramid fiber coated fabric |
| CN110982280A (en) * | 2019-12-24 | 2020-04-10 | 厦门汉升橡塑制品有限公司 | Flame-retardant silicone rubber and preparation method thereof |
| CN111188202A (en) * | 2020-02-10 | 2020-05-22 | 广州市新荔缘鞋业有限公司 | Flame-retardant high-temperature-resistant composite fabric and preparation method thereof |
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Cited By (12)
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| CN103687989A (en) * | 2012-07-19 | 2014-03-26 | 大宇国际株式会社 | Synthetic leather production method using different liquid silicone rubber coating solutions |
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| CN109667143A (en) * | 2018-12-19 | 2019-04-23 | 青岛天邦线业有限公司 | A kind of fiberglass threads impregnation RFL inorganic agent and preparation method thereof |
| CN110904691A (en) * | 2019-10-18 | 2020-03-24 | 安徽华烨特种材料有限公司 | Preparation process of organic silicon modified aramid fiber coated fabric |
| CN110982280A (en) * | 2019-12-24 | 2020-04-10 | 厦门汉升橡塑制品有限公司 | Flame-retardant silicone rubber and preparation method thereof |
| CN111188202A (en) * | 2020-02-10 | 2020-05-22 | 广州市新荔缘鞋业有限公司 | Flame-retardant high-temperature-resistant composite fabric and preparation method thereof |
| CN111188202B (en) * | 2020-02-10 | 2022-07-12 | 山东大统服饰有限责任公司 | Flame-retardant high-temperature-resistant composite fabric and preparation method thereof |
| CN113354939A (en) * | 2021-06-30 | 2021-09-07 | 湖北菲客体育产业集团有限公司 | Manufacturing method of silicon PU plastic track |
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Application publication date: 20120718 Assignee: BEIJING JIAHUATAI TECHNOLOGY CO., LTD. Assignor: Beijing Guanghua Textile Group Co. Ltd.|Beijing Zhongfang Haitian dyeing and Weaving Technology Co. Ltd. Contract record no.: 2016110000015 Denomination of invention: Preparation method for aramid fiber-organic silicon composite material Granted publication date: 20140416 License type: Exclusive License Record date: 20161008 |
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| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Beijing City Guanghua Building No. 8 Guanghua Road, Chaoyang District 100026 Co-patentee after: Beijing Zhongfang Haitian New Material Technology Co. Ltd. Patentee after: Beijing Guanghua Textile Group Co., Ltd. Address before: Beijing City Guanghua Building No. 8 Guanghua Road, Chaoyang District 100026 Co-patentee before: Beijing Zhongfang Haitian Dyeing And Weaving Technology Co., Ltd. Patentee before: Beijing Guanghua Textile Group Co., Ltd. |