CN108148329B - A kind of preparation method and product of modified polytetrafluoroethylene impregnation liquid - Google Patents
A kind of preparation method and product of modified polytetrafluoroethylene impregnation liquid Download PDFInfo
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- CN108148329B CN108148329B CN201711330543.XA CN201711330543A CN108148329B CN 108148329 B CN108148329 B CN 108148329B CN 201711330543 A CN201711330543 A CN 201711330543A CN 108148329 B CN108148329 B CN 108148329B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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Abstract
本发明涉及一种改性聚四氟乙烯浸渍液的制备方法，包括如下步骤：1)将蒙脱土加入到乙醇中，然后加入硅烷偶联剂，65‑85℃条件下反应3‑6h，冷却、过滤、干燥，得到中间物；2)将中间物加入到水中，然后加入N,N‑二甲基十二烷基二甲基叔胺，65‑85℃条件下反应3‑6h，冷却、过滤，得到改性蒙脱土；3)将聚四氟乙烯分散液加入到水中，然后加入改性蒙脱土，混合均匀，即得改性聚四氟乙烯浸渍液。该方法所制备的改性聚四氟乙烯浸渍液，可大幅度地提高聚四氟乙烯/玻璃纤维膜材的柔韧性、粘结强度、力学性能和耐折叠性，使其便于生产、运输和安装。
The invention relates to a method for preparing a modified polytetrafluoroethylene dipping solution, comprising the following steps: 1) adding montmorillonite into ethanol, then adding a silane coupling agent, and reacting at 65-85° C. for 3-6 hours, Cooling, filtering, drying to obtain the intermediate; 2) adding the intermediate to water, then adding N,N-dimethyldodecyldimethyl tertiary amine, reacting for 3-6h at 65-85°C, cooling and filtering to obtain modified montmorillonite; 3) adding the polytetrafluoroethylene dispersion into water, then adding the modified montmorillonite, and mixing evenly to obtain the modified polytetrafluoroethylene impregnating liquid. The modified polytetrafluoroethylene impregnation solution prepared by the method can greatly improve the flexibility, bonding strength, mechanical properties and folding resistance of the polytetrafluoroethylene/glass fiber membrane, making it convenient for production, transportation and operation. Install.
Description
Technical Field
The invention relates to the field of preparation of flexible membrane materials, in particular to a preparation method of a modified polytetrafluoroethylene impregnation liquid and a product.
Background
The polytetrafluoroethylene has the characteristics of super-hydrophobicity, self-cleaning, flame retardancy, corrosion resistance and the like, and is coated on the surface of the glass fiber fabric to produce various polytetrafluoroethylene/glass fiber membrane materials. And the fabric is a high-performance industrial textile used in the building industry, and is mainly used in various large buildings such as large stadiums, public entertainment and leisure squares, shopping centers and the like. With the construction of large stadiums such as the olympic games of beijing 2008, the world expo of 2010 shanghai, and the guangzhou asian games, the market demand of the polytetrafluoroethylene/glass fiber membrane material is continuously increasing.
However, due to the characteristics of brittleness and breakage of the glass fiber, and the fact that the polytetrafluoroethylene/glass fiber membrane material inevitably encounters bending or folding problems in the processes of production, transportation and installation, the strength of the membrane material after being folded has large loss, and the loss of mechanical properties is large along with the increase of the bending or folding times. In addition, polytetrafluoroethylene/glass fiber membranes prepared by impregnating polytetrafluoroethylene dispersions in the prior art have poor flexibility and are difficult to transport and construct, resulting in increased cost.
Therefore, the novel polytetrafluoroethylene impregnation liquid is developed to impregnate the glass fiber fabric so as to improve the strength and flexibility of the polytetrafluoroethylene/glass fiber membrane material, and has important economic value and social significance.
Disclosure of Invention
The invention aims to provide a preparation method of a modified polytetrafluoroethylene impregnation solution, aiming at overcoming the defects of the prior art, and the prepared modified polytetrafluoroethylene impregnation solution can greatly improve the flexibility, the bonding strength, the mechanical property and the folding resistance when being used for preparing a polytetrafluoroethylene/glass fiber membrane material.
The technical scheme provided by the invention is as follows:
a preparation method of a modified polytetrafluoroethylene impregnation liquid comprises the following steps:
1) adding montmorillonite into ethanol, adding a silane coupling agent, reacting for 3-6h at 65-85 ℃, cooling, filtering and drying to obtain an intermediate;
2) adding the intermediate into water, adding N, N-dimethyl dodecyl dimethyl tertiary amine, reacting for 3-6h at 65-85 ℃, cooling, and filtering to obtain modified montmorillonite;
3) and adding the polytetrafluoroethylene dispersion liquid into water, then adding the modified montmorillonite, and uniformly mixing to obtain the modified polytetrafluoroethylene impregnation liquid.
Because the silane coupling agent and the N, N-dimethyl dodecyl dimethyl tertiary amine are both small molecules, the migration and the precipitation are easy to occur in the matrix, which causes environmental pollution and damages to the mechanical properties of the material. Therefore, in the technical scheme, the silane coupling agent and the montmorillonite are subjected to surface hydroxyl reaction to generate the montmorillonite with silane groups, and then the montmorillonite is reacted with the N, N-dimethyl dodecyl dimethyl tertiary amine to generate the montmorillonite with the long molecular chain of the N, N-dimethyl dodecyl dimethyl tertiary amine. The above process has the following advantages: (1) the migration and the precipitation of a silane coupling agent and N, N-dimethyl dodecyl dimethyl tertiary amine are avoided; (2) because the N, N-dimethyl dodecyl dimethyl tertiary amine has excellent antibacterial performance, the montmorillonite containing the long molecular chain of the N, N-dimethyl dodecyl dimethyl tertiary amine has permanent antibacterial performance; (3) the modified montmorillonite can be uniformly dispersed in the aqueous solution, the agglomeration and precipitation phenomena are avoided, and the compatibility of the obtained modified montmorillonite and a matrix is excellent.
Preferably, the mass ratio of the montmorillonite to the ethanol in the step 1) is 1: 3-10.
Preferably, the montmorillonite in the step 1) is sodium montmorillonite, calcium montmorillonite or magnesium montmorillonite.
Preferably, the mass ratio of the silane coupling agent to the montmorillonite in the step 1) is 1: 1-10.
Preferably, the silane coupling agent in the step 1) is one or more of KH550, KH560 and KH 570.
Preferably, the mass ratio of the intermediate to the water in the step 2) is 1: 1-10.
Preferably, the mass ratio of the intermediate in the step 2) to the N, N-dimethyl dodecyl dimethyl tertiary amine is 1: 1-10.
Preferably, the mass ratio of the modified montmorillonite to the polytetrafluoroethylene dispersion liquid in the step 3) is 1: 50-100.
Preferably, the mass ratio of the water to the polytetrafluoroethylene dispersion in the step 3) is 1: 0.5-10.
Preferably, the polytetrafluoroethylene dispersion liquid in the step 3) is one or more of polytetrafluoroethylene TE3859 type, F-104 type, FR303A type, FR302 type and DF311 type.
Preferably, the preparation method of the modified polytetrafluoroethylene impregnation liquid comprises the following steps:
1) adding montmorillonite into ethanol, adding a silane coupling agent, reacting for 3-6h at 65-85 ℃, cooling, filtering and drying to obtain an intermediate; the mass ratio of the montmorillonite to the ethanol is 1: 3-3.5; the montmorillonite is sodium montmorillonite; the mass ratio of the silane coupling agent to the montmorillonite is 1: 1-1.5; the silane coupling agent is KH550 silane coupling agent;
2) adding the intermediate into water, adding N, N-dimethyl dodecyl dimethyl tertiary amine, reacting for 3-6h at 65-85 ℃, cooling, and filtering to obtain modified montmorillonite; the mass ratio of the intermediate to the water is 1: 2.5-3.5; the mass ratio of the intermediate to the N, N-dimethyl dodecyl dimethyl tertiary amine is 1: 1-1.5;
3) adding the polytetrafluoroethylene dispersion liquid into water, then adding the modified montmorillonite, and uniformly mixing to obtain a modified polytetrafluoroethylene impregnation liquid; the mass ratio of the modified montmorillonite to the polytetrafluoroethylene dispersion liquid is 1: 50-55; the mass ratio of the water to the polytetrafluoroethylene dispersion liquid is 1: 0.5-0.7; the polytetrafluoroethylene dispersion is of a polytetrafluoroethylene TE3859 type.
The invention also provides the modified polytetrafluoroethylene impregnation liquid prepared by the preparation method.
Compared with the prior art, the invention has the beneficial effects that:
(1) the modified montmorillonite in the modified polytetrafluoroethylene impregnation liquid prepared by the invention is uniformly dispersed, is not easy to agglomerate and has good stability.
(2) The modified polytetrafluoroethylene impregnation liquid prepared by the invention takes water as a solvent, and avoids volatilization of a large amount of toxic solvent, and pollution to the surrounding environment and human health.
(3) The modified polytetrafluoroethylene impregnating solution prepared by the invention can greatly improve the flexibility and folding resistance of the polytetrafluoroethylene/glass fiber membrane material, and is convenient for production, transportation and installation.
Drawings
FIG. 1 is an optical microscopic view of a modified polytetrafluoroethylene impregnation solution prepared in example 1;
FIG. 2 is an optical microscope photograph of a modified polytetrafluoroethylene impregnation solution prepared in example 5;
FIG. 3 is an optical microscope photograph of a modified polytetrafluoroethylene impregnation solution prepared in example 6;
FIG. 4 is an optical microscope photograph of a polytetrafluoroethylene impregnation solution prepared in comparative example 2;
FIG. 5 is an optical microscope photograph of a polytetrafluoroethylene impregnation solution prepared in comparative example 3;
FIG. 6 is an optical microscope photograph of a polytetrafluoroethylene impregnation solution prepared in comparative example 4;
FIG. 7 is an SEM image of a PTFE/fiberglass membrane made from example 1;
FIG. 8 is an SEM image of a PTFE/fiberglass membrane made from example 5;
FIG. 9 is an SEM image of a PTFE/fiberglass membrane made in example 6;
FIG. 10 is an SEM image of a PTFE/fiberglass membrane made from comparative example 1;
FIG. 11 is an SEM image of a polytetrafluoroethylene/glass fiber membrane made from comparative example 2;
FIG. 12 is an SEM image of a polytetrafluoroethylene/glass fiber membrane made from comparative example 3;
fig. 13 is an SEM image of a polytetrafluoroethylene/glass fiber membrane prepared from comparative example 4.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
1) Firstly, 100g of sodium-based montmorillonite is added into 95 wt% ethanol (the mass ratio of the sodium-based montmorillonite to the ethanol is 1/3), then KH560 silane coupling agent is added (the mass ratio of the KH560 to the sodium-based montmorillonite is 1/1), the mixture reacts for 3 hours at the temperature of 80 ℃, and the intermediate is obtained after cooling, filtering and drying;
2) adding the intermediate into deionized water (the mass ratio of the intermediate to the water is 1/3), adding N, N-dimethyl dodecyl dimethyl tertiary amine (the mass ratio of the intermediate to the N, N-dimethyl dodecyl dimethyl tertiary amine is 1/1), reacting for 3h at 80 ℃, cooling, and filtering to obtain the modified montmorillonite.
3) Adding TE3859 type polytetrafluoroethylene dispersion liquid into deionized water (the mass ratio of water to polytetrafluoroethylene is 1/0.66), then adding modified montmorillonite (the mass ratio of modified montmorillonite to polytetrafluoroethylene is 1/50), and uniformly mixing at 25 ℃ to obtain 40 wt% modified polytetrafluoroethylene impregnation liquid.
The modified polytetrafluoroethylene impregnation solution prepared in example 1 was subjected to optical microscopy characterization, as shown in fig. 1.
Example 2
Preparation was carried out with reference to example 1 except that the mass ratio of water to polytetrafluoroethylene was 1/1.5, to obtain a 60 wt% modified polytetrafluoroethylene impregnation solution.
Example 3
The preparation was carried out with reference to example 1, except that the mass ratio of sodium-based montmorillonite to ethanol was 1/5. The mass ratio of the KH560 to the Na-montmorillonite is 1/5. The mass ratio of intermediate to water was 1/5. The mass ratio of the intermediate to N, N-dimethyldodecyldimethyl tertiary amine was 1/5. The mass ratio of the modified montmorillonite to the polytetrafluoroethylene is 1/75, and the modified polytetrafluoroethylene impregnation liquid is obtained.
Example 4
The preparation was carried out with reference to example 1, except that the mass ratio of sodium-based montmorillonite to ethanol was 1/10. The mass ratio of the KH560 to the Na-montmorillonite is 1/10. The mass ratio of intermediate to water was 1/10. The mass ratio of the intermediate to N, N-dimethyldodecyldimethyl tertiary amine was 1/10. The mass ratio of the modified montmorillonite to the polytetrafluoroethylene is 1/100, and the modified polytetrafluoroethylene impregnation liquid is obtained.
Example 5
The preparation was carried out with reference to example 1, except that sodium montmorillonite was changed to calcium montmorillonite to obtain a modified polytetrafluoroethylene impregnation solution.
The modified polytetrafluoroethylene impregnation solution prepared in example 5 was subjected to optical microscopy characterization, as shown in fig. 2.
Example 6
The preparation was carried out as described in reference example 1, except that sodium-based montmorillonite was changed to magnesium-based montmorillonite to obtain a modified polytetrafluoroethylene impregnation solution.
The modified polytetrafluoroethylene impregnation solution prepared in example 6 was subjected to optical microscopy characterization, as shown in fig. 3.
Comparative example 1
Pure polytetrafluoroethylene dispersion of type TE3859 was used.
Comparative example 2
Adding TE3859 type polytetrafluoroethylene dispersion into deionized water (the mass ratio of water to polytetrafluoroethylene is 1/0.66), then adding sodium-based montmorillonite (the mass ratio of sodium-based montmorillonite to polytetrafluoroethylene is 1/50), and uniformly mixing at 25 ℃ to obtain 40 wt% polytetrafluoroethylene impregnation liquid.
The optical microscope characterization was performed on the polytetrafluoroethylene impregnation solution prepared in comparative example 2, as shown in fig. 4.
Comparative example 3
Adding TE3859 type polytetrafluoroethylene dispersion liquid into deionized water (the mass ratio of water to polytetrafluoroethylene is 1/0.66), then adding calcium-based montmorillonite (the mass ratio of calcium-based montmorillonite to polytetrafluoroethylene is 1/50), and uniformly mixing at 25 ℃ to obtain 40 wt% polytetrafluoroethylene impregnation liquid.
The optical microscope characterization was performed on the polytetrafluoroethylene impregnation solution prepared in comparative example 3, as shown in fig. 5.
Comparative example 4
Adding TE3859 type polytetrafluoroethylene dispersion into deionized water (the mass ratio of water to polytetrafluoroethylene is 1/0.66), then adding magnesium-based montmorillonite (the mass ratio of magnesium-based montmorillonite to polytetrafluoroethylene is 1/50), and uniformly mixing at 25 ℃ to obtain 40 wt% polytetrafluoroethylene impregnation liquid.
The optical microscope characterization was performed on the polytetrafluoroethylene impregnation solution prepared in comparative example 4, as shown in fig. 6.
Performance testing
Firstly, soaking the glass fiber fabric in the polytetrafluoroethylene soaking solution obtained in the examples 1-6 and the comparative examples 1-4, and then drying at 150 ℃ for 60s, at 280 ℃ for 60s and at 380 ℃ for 60s to obtain the polytetrafluoroethylene/glass fiber membrane material.
SEM characteristics are respectively carried out on the polytetrafluoroethylene/glass fiber membrane materials prepared in the examples 1, 5 and 6 and the comparative examples 1 to 4, and as shown in figures 7 to 13, the cross-sectional shapes of the polytetrafluoroethylene/glass fiber membrane materials prepared in the examples 1, 5 and 6 are stacked in a sheet shape, the sections are densely stacked with each other, and the mechanical strength and the flexibility can be greatly improved as compared with the traditional brick-tile structure.
As shown by the section shapes of the polytetrafluoroethylene/glass fiber membranes prepared in the comparative examples 1-4, the glass fiber and the polytetrafluoroethylene have poor bonding strength and are in a separated state, so that the mechanical strength and the flexibility can not be greatly improved.
The folding endurance was further measured by rolling a polytetrafluoroethylene/glass fiber film material in a reciprocating manner with a steel roller having a mass of 4.5kg and a diameter of 90mm 0, 10, 20, 30, 40, 50 times in accordance with ASTM D4851 standard, and then measuring the breaking strength, and the results are shown in Table 1.
Table 1 shows the breaking strength comparison of the polytetrafluoroethylene/glass fiber membranes prepared in examples 1 to 6 and comparative examples 1 to 4
"-" indicates that the sample had fractured before testing and could not be further tested.
The polytetrafluoroethylene/glass fiber membrane was tested for folding resistance using a folding resistance tester, as shown in table 2 below.
Table 2 shows the folding endurance of the polytetrafluoroethylene/glass fiber membranes prepared in examples 1 to 6 and comparative examples 1 to 4
The experimental results in tables 1 and 2 show that the modified polytetrafluoroethylene impregnation liquid obtained in examples 1 to 6 of the preparation method of the invention can greatly improve the flexibility, bonding strength, mechanical properties and folding resistance of the polytetrafluoroethylene/glass fiber membrane material, and is convenient for production, transportation and installation.
Claims (7)
1. The preparation method of the modified polytetrafluoroethylene impregnation liquid is characterized by comprising the following steps:
1) adding montmorillonite into ethanol, adding a silane coupling agent, reacting for 3-6h at 65-85 ℃, cooling, filtering and drying to obtain an intermediate; the mass ratio of the silane coupling agent to the montmorillonite is 1: 1-10;
2) adding the intermediate into water, adding dodecyl dimethyl tertiary amine, reacting for 3-6h at 65-85 ℃, cooling, and filtering to obtain modified montmorillonite; the mass ratio of the intermediate to the dodecyl dimethyl tertiary amine is 1: 1-10;
3) and adding the polytetrafluoroethylene dispersion liquid into water, then adding the modified montmorillonite, and uniformly mixing to obtain the modified polytetrafluoroethylene impregnation liquid.
2. The method for preparing the modified polytetrafluoroethylene impregnating solution according to claim 1, wherein the mass ratio of the montmorillonite to the ethanol in the step 1) is 1: 3-10.
3. The method for preparing a modified polytetrafluoroethylene impregnating solution according to claim 1, wherein the montmorillonite in step 1) is sodium-based montmorillonite, calcium-based montmorillonite or magnesium-based montmorillonite.
4. The method for preparing a modified polytetrafluoroethylene impregnating solution according to claim 1, wherein the mass ratio of the intermediate to water in step 2) is 1: 1-10.
5. The method for preparing the modified polytetrafluoroethylene impregnating solution according to claim 1, wherein the mass ratio of the modified montmorillonite to the polytetrafluoroethylene dispersion solution in the step 3) is 1: 50-100.
6. The method for preparing a modified polytetrafluoroethylene impregnating solution according to claim 1, wherein the mass ratio of water to the polytetrafluoroethylene dispersion in said step 3) is 1: 0.5-10.
7. The modified polytetrafluoroethylene impregnating solution prepared by the preparation method according to any one of claims 1 to 6.
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| CN1379798A (en) * | 1999-10-21 | 2002-11-13 | 大金工业株式会社 | Resin articles for molding and process for producing same |
| CN102206399A (en) * | 2011-04-15 | 2011-10-05 | 广东生益科技股份有限公司 | Composition for copper-clad laminate with low dielectric constant and copper-clad laminate manufactured by using same |
| CN106751711A (en) * | 2017-01-18 | 2017-05-31 | 腾辉电子（苏州）有限公司 | Fluorine substituted ethylene based polyalcohol resin combination, prepreg and laminate |
| CN106854330A (en) * | 2016-11-25 | 2017-06-16 | 常州中英科技股份有限公司 | A kind of fluorine resin mixture and its prepreg and the copper-clad plate of preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1379798A (en) * | 1999-10-21 | 2002-11-13 | 大金工业株式会社 | Resin articles for molding and process for producing same |
| CN102206399A (en) * | 2011-04-15 | 2011-10-05 | 广东生益科技股份有限公司 | Composition for copper-clad laminate with low dielectric constant and copper-clad laminate manufactured by using same |
| CN106854330A (en) * | 2016-11-25 | 2017-06-16 | 常州中英科技股份有限公司 | A kind of fluorine resin mixture and its prepreg and the copper-clad plate of preparation |
| CN106751711A (en) * | 2017-01-18 | 2017-05-31 | 腾辉电子（苏州）有限公司 | Fluorine substituted ethylene based polyalcohol resin combination, prepreg and laminate |
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