CN102808326B - Preparation method for modified inorganic fiber cloth - Google Patents
Preparation method for modified inorganic fiber cloth Download PDFInfo
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- CN102808326B CN102808326B CN201210287644.4A CN201210287644A CN102808326B CN 102808326 B CN102808326 B CN 102808326B CN 201210287644 A CN201210287644 A CN 201210287644A CN 102808326 B CN102808326 B CN 102808326B
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Abstract
The invention relates to a preparation method for modified inorganic fiber cloth. The preparation method comprises the steps as follows: firstly, removing a soaking agent on inorganic fiber cloth; secondly, soaking the inorganic fiber cloth in a surface treating agent; and lastly, drying and baking to obtain the modified inorganic fiber cloth, wherein the surface treating agent is prepared by uniformly mixing the following components: 5-40 wt% of PTFE (polytetrafluoroethylene), 0.05-5 wt% of rare earth surface modifier, 0.5-5 wt% of fluorine-containing three-proofing finishing agent, 0.01-2 wt% of dispersion stabilizer, 0.1-5 wt% of penetrating agent and the balance of water. According to the preparation method, the bonding performance of the PTFE and the inorganic fiber surface is improved by the rare earth surface modification technology, and the prepared inorganic fiber cloth has the advantages of more excellent surface coating state, better corrosion resistance, mechanical property, fold resistance and wear resistance, and longer service life.
Description
Technical field
The present invention relates to a kind of preparation method of modified inorganic cloth, belong to fine chemical technology field.
Background technology
Coupling agent can be divided into Organic Chromium complex compound, silanes, titanate ester and the large class of aluminic acid compound four by chemical constitution and composition.Domestic inorfil industry extensively adopts silane coupler to be used as the surface modifier of interface performance between inorfil and polytetrafluoroethylene (PTFE), because the inertia of PTFE causes the modified effect of silane coupler limited, cause the coating on inorfil surface to be not in good state, the heatproof of inorfil cloth, anticorrosive, mechanical property, folding mill performance are limited, are therefore also restricting inorfil cloth service life.
For silane coupler, first, silane coupler hydrolysis, generates silanol, and inorfil water absorbent surface, generates hydroxyl simultaneously; Then the inorfil Surface Creation hydrogen bond of silanol and water suction; Drying and dehydrating at low temperatures, makes to occur between silanol etherification reaction; Then drying and dehydrating at high temperature, makes silanol and water suction inorfil carry out etherification reaction, and silane coupler and inorfil surface conjunction get up like this.R group in silane coupler will be with PTFE by the diffusion mode formation network structure of mutually entwining, extremely strong fluorine atom and the lone pair electrons in coupling agent R group of electronegativity form coordinate bond under specific circumstances, reason due to fluorine atom inertia, the formation of coordinate bond is limited, play like this effect that improves inorfil and PTFE Interface adhesive strength, here physical action is occupied an leading position, rather than the effect of chemical bond, and the effect of visible silane coupler interface modification is limited.Simultaneously silane coupler is limited in heat resistance, be greater than under the high temperature of 200 ℃ easily aging.
Summary of the invention
The object of the invention is for using conventional silane coupler to prepare the defect that inorfil cloth brings, a kind of preparation method of modified inorganic cloth is provided, the inorfil cloth that makes is improved at aspect of performances such as heatproof, anticorrosive, mechanics, folding mills, also improves inorfil cloth life-span and result of use in actual applications simultaneously.
Technical scheme of the present invention is: first remove the sizing agent on inorfil cloth, then inorfil cloth be impregnated in surface conditioning agent, finally by being dried, curing, obtain.
Described surface conditioning agent, is mixed and be get final product by following component: 5 ~ 40wt%PTFE(ptfe emulsion), and 0.05 ~ 5wt% RE surface modifying agent, the fluorine-containing three-proof finishing agent of 0.5 ~ 5wt%, 0.01 ~ 2wt% dispersion stabilizer, 0.1 ~ 5wt% bleeding agent, surplus is water.
Described inorfil cloth is preferably glass fabric or basalt fiber cloth.Other inorfil cloth also available this method carries out modification, but glass fabric and basalt fiber cloth are the most frequently used, best results.
The method of the sizing agent on described removal inorfil cloth is selected from: hot cleaning, washing or smoldering.The common method of removing sizing agent is heat treatment and WATER-WASHING METHOD, heat treating process is more conventional, it comprises heat cleaning (continuous treatment process) and smoldering (batch process method), it is the inorfil cloth short time by high temperature, to remove continuously the method for sizing agent that heat is cleaned, and smoldering is that inorfil cloth is placed in to the method for removing sizing agent under certain high temperature for a long time.
As preferably, it is 0.5 ~ 5min that inorfil cloth impregnated in the time in surface conditioning agent.Dip time meets the demands within the scope of this, and overlong time does not have practical significance.
Described baking temperature is 100 ~ 250 ℃, and the time is 2 ~ 10min.Dry object is to make moisture evaporation.Temperature and time is controlled within the scope of this can obtain good drying effect.
Described stoving temperature is 180 ~ 300 ℃, and the time is 2 ~ 15min.The object of curing is the active principle full and uniform film forming at high temperature that makes surface conditioning agent.
In above-mentioned surface treatment agent prescription, PTFE can improve chemical resistance, folding mill property, hydrophobicity and the service life of inorfil cloth.
Described RE surface modifying agent is the compound of lanthanum, cerium, and it can obviously improve the binding ability of inorganic-organic interface; As preferably, described RE surface modifying agent is selected from one or more mixtures that form with arbitrary proportion in lanthana, cerium oxide, lanthanum nitrate, cerous nitrate, lanthanum chloride or cerium chloride.These compound prices are low, easily obtain, and surface modification effect is good.
Described fluorine-containing three-proof finishing agent is that this area is conventional, commercially available acquisition, the precious series of Austria profit fluorine of Ru du pont company (model has sharp fluorine difficult to understand precious OC, Oleophobol C P-SLA, the precious SLA-NEW of sharp fluorine difficult to understand, sharp fluorine treasured 7713 difficult to understand etc.), the effect of fluorine-containing three-proof finishing agent is the hydrophobic that improves inorfil cloth, hates oil and service life.
The preferred non-ion fluorin carbon surface active agent of described dispersion stabilizer, non-ion fluorin carbon surface active agent is well known in the art and conventional, commercially available acquisition, as the FSN of E.I.Du Pont Company series (as FSN-100), FSG series (as FSG) and FSO series (as FSO-100).The effect of dispersion stabilizer is stability of emulsion and the dispersiveness that improves surface conditioning agent.
The preferred polyoxyethylene non-ionic surface active agent of described bleeding agent, polyoxyethylene non-ionic surface active agent is bleeding agent well known in the art, commercial can acquisition, for example, the penetrating agent JFC series (model has JFC, JFC-1, JFC-2, JFC-E etc.) that the Jia Feng of Jiangsu Province chemistry limited company produces, the effect of bleeding agent is the surface tension of surface conditioning agent that significantly declines, while making to flood surface conditioning agent, can efficiently enter inorfil cloth yarn inner, to carrying out modification thoroughly inside and outside inorfil cloth.
The present invention selects RE surface modifying agent to compare conventional coupling agent, as silane coupler, titanate coupling agent etc., has higher heat resistance, and RE surface modifying agent is better than conventional coupling agent for the improvement of inorfil and PTFE binding ability.Because rare earth has special 4f layer structure and the less characteristic of electronegativity, make it have outstanding chemism.As the rare earth element of surface active element, when surface treatment, be first adsorbed on fiber surface, system capacity is reduced.After absorption, a part of rare earth element is because its electronegativity value is low, and it is by the oxygen of capturing in inorfil surface hydroxyl, and the main component of inorfil is SiO
2with metal oxide, and at inorfil surface SiO
2, Al
2o
3content relatively many, thereby improve the interface binding power between inorfil and matrix.The 4f duplet atomic nucleus bad sealing of rare earth atom, shows larger effective nuclear charge.Electronics to atom around it has stronger attraction.At rare earth element and PTFE interface, the formed RE-F key of rare earth element or RE-C key have stronger ion key.Meanwhile, be present in the rare earth compound of interface, played the effect that is similar to " pinning ", strengthen the mechanical adhesion between inorfil and PTFE, further improved the compatibility between inorfil and PTFE matrix.
Above-mentioned surface treatment mechanism is:
(1) inorfil cloth is removed the organic matters such as sizing agent on it by methods such as hot cleaning, smoldering or washings, for surface conditioning agent carries out modification to inorfil, provides clean interface.
(2), after treated dose of dipping of inorfil cloth, surface forms one with the mixed uniformly emulsion film of granule form, the RE surface modifying agent in inorfil surface attachment finishing agent.
(3), in body of heater, because the evaporation of moisture causes the emulsion film attenuation gradually on inorfil surface, granule precipitates gradually, on the surface of inorfil, has formed one deck macromolecule membrane.
(4) under the effect of high temperature; moisture further evaporates; between surface modifier and inorfil surface, occur to combine with chemical bond; rare-earth surface modification and PTFE are with ionic bond and mechanical adhesion; " bridge " effect of RE surface modifying agent plays inorganic-organic interface; strengthen the adhesive property between inorfil and organic matter, between the granule of the organic components deposit buildup in surface conditioning agent, melting mutually, forms good polymer protective film.
The present invention is the modified effect for inorfil cloth by the agent of rare-earth surface modification technology enhanced surface treatment, and the rare earth compound of selecting is water-solubility rare-earth compound, configures simplely, and inorfil and PTFE interfacial combined function are improved to successful; By the acting in conjunction of dispersion stabilizer and bleeding agent, finishing agent stable performance, can fully infiltrate inorfil cloth inner, made up the conventional technology of preparing of inorfil cloth apply conventional coupling agent exist high temperature easily aging, inorfil is combined to modified effect with PTFE a little less than, the deficiency such as, mechanics anticorrosive to inorfil, the enhancing of folding mill performance be limited, there is high efficiency, low cost, environmental friendliness, simple for process, can obviously improve the coating state of inorfil and PTFE and apply effect, interfacial combined function is fully improved.The actual heatproof of the inorfil cloth filtrate making by the inventive method, anticorrosive, mechanics, the performance test performance such as wear-resisting improve all more than 20%.
The specific embodiment
Below in conjunction with instantiation, the invention will be further described.
Embodiment 1
Prepare surface conditioning agent:
| Component | Mass percent, % |
| PTFE | 25 |
| Lanthanum chloride | 0.3 |
| Finishing agent sharp fluorine treasured 7713 difficult to understand | 2 |
| Dispersion stabilizer FSN-100 | 1 |
| Penetrating agent JFC | 1 |
| Water | Surplus |
Said components is mixed, obtain surface conditioning agent.
Employing is at 90 ℃, in the amylase solution of 3wt%, the method for washing of Ultrasonic Cleaning 5min is removed the sizing agent on glass fabric, then glass fabric be impregnated in to 1min in surface conditioning agent, finally dry 2min at 180 ℃ of temperature, at 260 ℃ of temperature, cure 10min, obtain.
Embodiment 2
Prepare surface conditioning agent:
| Component | Mass percent, % |
| PTFE | 5 |
| Cerous nitrate | 4 |
| The precious OC of the difficult to understand sharp fluorine of finishing agent | 1 |
| Dispersion stabilizer FSO-100 | 0.5 |
| Penetrating agent JFC-1 | 0.5 |
| Water | Surplus |
Said components is mixed, obtain surface conditioning agent.
Employing keeps the smoldering method of 24h to remove the sizing agent on glass fabric at 250 ℃, then glass fabric be impregnated in to 0.5min in surface conditioning agent, and finally dry 4min at 200 ℃ of temperature cures 8min at 280 ℃ of temperature, obtains.
Embodiment 3
Prepare surface conditioning agent:
| Component | Mass percent, % |
| PTFE | 40 |
| Lanthanum chloride | 0.05 |
| Cerous nitrate | 0.05 |
| The precious SLA-NEW of difficult to understand sharp fluorine | 4 |
| Dispersion stabilizer FSO-100 | 0.01 |
| Penetrant JFC-2 | 4 |
| Water | Surplus |
Said components is mixed, obtain surface conditioning agent.
Employing keeps the hot cleaning method of 45s to remove the sizing agent on basalt fiber cloth at 400 ℃, then basalt fiber cloth be impregnated in to 3min in surface conditioning agent, and finally dry 5min at 220 ℃ of temperature cures 15min at 260 ℃ of temperature, obtains.
Comparative example
Prepare surface conditioning agent:
Said components is mixed, obtain surface conditioning agent.
Employing keeps the hot cleaning method of 45s to remove the sizing agent on glass fabric at 400 ℃, then glass fabric be impregnated in to 2min in surface conditioning agent, and finally dry 2min at 180 ℃ of temperature cures 10min at 260 ℃ of temperature, obtains.
Performance test:
The inorfil cloth that embodiment and comparative example are made is by surperficial SEM electron microscopic observation, and carry out heatproof, corrosion-resistant, folding anti-wear performance and Mechanics Performance Testing contrast, the method of testing of heat resistance, folding quality, anti-wear performance and mechanical property is with reference to GB/T6719-2009, decay resistance test comprises acid proof test and alkaline-resisting test, and acid proof test is the H at 2.5wt%
2sO
4in solution, place 24h, alkaline-resisting test for to place 24h in the NaOH of 5wt% solution.
Test result sees the following form:
Test result shows: the modified inorganic cloth that the present invention makes is all being better than the inorfil cloth that conventional coupling agent makes aspect finishing agent surface coating state, heatproof, corrosion-resistant, folding mill performance and mechanical property.
Claims (5)
1. a preparation method for modified inorganic cloth, is characterized in that, first removes the sizing agent on inorfil cloth, then inorfil cloth be impregnated in surface conditioning agent, finally by being dried, curing, obtains;
Described surface conditioning agent, is mixed and be get final product by following component: 5～40wt%PTFE, and 0.05～5wt% RE surface modifying agent, the fluorine-containing three-proof finishing agent of 0.5～5wt%, 0.01～2wt% dispersion stabilizer, 0.1～5wt% bleeding agent, surplus is water;
Described inorfil cloth is glass fabric or basalt fiber cloth;
Described RE surface modifying agent is selected from one or more mixtures that form with arbitrary proportion in lanthanum nitrate, cerous nitrate, lanthanum chloride or cerium chloride.
2. the preparation method of modified inorganic cloth as claimed in claim 1, is characterized in that, the method for removing the sizing agent on inorfil cloth is selected from: hot cleaning, washing or smoldering.
3. the preparation method of modified inorganic cloth as claimed in claim 1, is characterized in that, it is 0.5～5min that inorfil cloth impregnated in the time in surface conditioning agent.
4. the preparation method of modified inorganic cloth as claimed in claim 1, is characterized in that, described baking temperature is 100～250 ℃, and the time is 2～10min.
5. the preparation method of modified inorganic cloth as described in claim 1 to 4 any one, is characterized in that, described stoving temperature is 180～300 ℃, and the time is 2～15min.
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| CN201210287644.4A CN102808326B (en) | 2012-08-13 | 2012-08-13 | Preparation method for modified inorganic fiber cloth |
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| CN102808326B true CN102808326B (en) | 2014-11-26 |
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| CN103877785B (en) * | 2012-12-24 | 2015-11-18 | 厦门三维丝环保股份有限公司 | Modification processing method before non-thermal plasticity chemical fibre filtrate overlay film |
| CN104448826A (en) * | 2014-10-28 | 2015-03-25 | 桐乡市科力复合材料有限公司 | Preparation method of polyphenylene sulfide, polytetrafluoroethylene and glass fiber cloth film-shaped ternary composite material |
| CN108285641A (en) * | 2018-02-05 | 2018-07-17 | 公牛集团股份有限公司 | A kind of modified glass-fiber, the nylon composite materials and its preparation method and application containing the modified glass-fiber |
| CN109232981A (en) * | 2018-07-18 | 2019-01-18 | 安徽江淮汽车集团股份有限公司 | A kind of modified diabase fiber and preparation method thereof |
| CN109778543A (en) * | 2019-01-14 | 2019-05-21 | 广西梧州市百裕实业有限公司 | A kind of three proofings school uniform and preparation method thereof |
| CN110898529A (en) * | 2019-12-17 | 2020-03-24 | 中材科技膜材料（山东）有限公司 | Smoke filtering composite filter material for glass melting furnace |
| CN112011926A (en) * | 2020-07-09 | 2020-12-01 | 南京龙源环保有限公司 | Needled felt filter material, surface treating agent and surface treating process thereof |
| CN112337190A (en) * | 2020-10-19 | 2021-02-09 | 南京玻璃纤维研究设计院有限公司 | Modified filter material and preparation method thereof |
| CN115094543A (en) * | 2022-06-17 | 2022-09-23 | 天津斯坦利新型材料有限公司 | Inorganic fiber, preparation method and semi-aromatic nylon composition prepared from inorganic fiber |
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| CN101781444A (en) * | 2010-03-31 | 2010-07-21 | 上海交通大学 | Method for preparing rare-earth-modified glass-fiber epoxy-resin composite materials |
| CN102151435B (en) * | 2011-01-27 | 2013-05-15 | 南京际华三五二一特种装备有限公司 | Glass fiber filter material and preparation method thereof |
| CN102392355A (en) * | 2011-09-27 | 2012-03-28 | 江苏鼎盛滤袋有限公司 | Preparation method for water-repelling grease-proofing easy-ash-removal filter material |
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Effective date of registration: 20200224 Address after: 210000 No.30, Andri, Yuhua West Road, Nanjing, Jiangsu Province Patentee after: Nanjing Glass Fibre Research and Design Institute company limited Address before: Jiangning District of Nanjing City, Jiangsu province 211100 Jiangning Science Park Tong Road No. 99 Patentee before: Sinoma Science & Technology Co.,Ltd. |