CN105061957A - Method for preparing modified calcium carbonate filled polytetrafluoroethylene composite - Google Patents
Method for preparing modified calcium carbonate filled polytetrafluoroethylene composite Download PDFInfo
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- CN105061957A CN105061957A CN201510518970.5A CN201510518970A CN105061957A CN 105061957 A CN105061957 A CN 105061957A CN 201510518970 A CN201510518970 A CN 201510518970A CN 105061957 A CN105061957 A CN 105061957A
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- calcium carbonate
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Abstract
The invention discloses a method for preparing a modified calcium carbonate filled polytetrafluoroethylene composite. The method comprises the steps that calcium carbonate, water, absolute ethyl alcohol, paraffin and antioxygen 1010 are mixed and stirred, and heating reflux, cooling and drying are carried out to obtain modified calcium carbonate powder; the modified calcium carbonate powder and polytetrafluoroethylene suspension powder are stirred and blended to obtain a mixture, the mixture is placed in a mold to be cooled and formed, and a composite board is obtained; the composite board is wrapped by aluminum foil to be placed in a muffle furnace, segmented temperature rising sintering is carried out according to the program, and the modified calcium carbonate filled polytetrafluoroethylene composite is obtained. According to the new process, cheap and easily-obtained calcium carbonate is modified and then filled with high-performance expensive polytetrafluoroethylene, corresponding performance is obtained, and meanwhile cost is greatly reduced. Compared with an unmodified calcium carbonate filled polytetrafluoroethylene composite, the elongation at break and tensile strength are greatly increased.
Description
Technical field
The invention belongs to field of compound material, be specifically related to a kind of preparation method of modified calcium carbonate filled polytetrafluoroethylene matrix material.
Background technology
Tetrafluoroethylene (PTFE) has excellent chemical stability, radioresistance, dielectric properties, pole low-friction coefficient and self lubricity, has important application in national economy fields such as chemical industry, machinery, electronics, electrical equipment, military project, space flight, environmental protection and bridges.But due to the constructional feature of PTFE molecule, between macromole, magnetism is less, and zoned crystal is easily peeled off by sheet, thus shows as poor mechanical property, linear expansivity and the shortcoming such as load metamorphism is large.The inorganic particle filled modified ptfes such as usual employing micron order graphite, molybdenumdisulphide, copper powder, glass fibre.
Mineral filler has high-modulus, the advantages such as easy preparation, its filling-modified polymer is a kind of method simply effectively improving high molecular chemical characters, calcium carbonate (comprising coarse whiting and fine particle calcium carbonate) has the plurality of advantages such as raw material is easy to get, cheap, good stability, color and luster are simple, nontoxic, and be widely used in the fields such as plastics, rubber, papermaking, ink, building materials, electric wire, be a kind of mineral filler being often used to filling-modified macromolecular material.Relative to PTFE synthetic resins, the price of calcium carbonate is much lower, is joined by calcium carbonate in PTFE, can improve the performance such as modulus and wear resistance of PTFE, also obviously can reduce the price of PTFE goods.Simultaneously compared to using the high cost of the inorganic particulate such as molybdenumdisulphide, copper powder filling-modified, the cost of calcium carbonate is obviously much low.But belong to inorganic powder due to calcium carbonate, particle surface is hydrophilic oleophobic, present stronger polarity, and bonding force is low between PTFE matrix, when the loading level height of calcium carbonate in PTFE matrix, the matrix material formed, when by external impacts, easily causes boundary defect, causes material property sharply to decline; Therefore, only have to calcium carbonate carry out suitable modification could meet in PTFE matrix, have larger loading level while and significantly can not reduce the mechanical strength of PTFE.
Generally speaking the powder surface modification of calcium carbonate selects titanate coupling agent, aluminate coupling agent mostly, and other tensio-active agent composite, dispersion agent and auxiliary agent etc. carry out surface modification.But in view of the higher moulding process requirement of tetrafluoroethylene, most of above-mentioned properties-correcting agent all can not meet the effect of low cost, high-level efficiency modified calcium carbonate.
Summary of the invention
The object of the invention is the modified calcium carbonate filled polytetrafluoroethylene composite material and preparation method thereof providing a kind of excellent performance, low cost.
For achieving the above object, adopt technical scheme as follows:
The preparation method of modified calcium carbonate filled polytetrafluoroethylene matrix material, comprises the following steps:
By calcium carbonate, water, dehydrated alcohol, paraffin, antioxidant 1010 mix and blend, reflux, cooling, oven dry obtain modified calcium carbonate powder;
Above-mentioned modified calcium carbonate powder and polytetrafluoroethylsuspending suspending powder blended under agitation are obtained compound, compound is put into mold cold pressing formation and obtain composite sheet;
Wrap as in retort furnace with aluminium foil by described composite sheet, program segmenting heats up and sinters, and obtains modified calcium carbonate filled polytetrafluoroethylene matrix material.
By such scheme, described raw materials by weight portion meter is as follows:
By such scheme, described program segmenting intensification sintering process is as follows:
First stage rises to 180 DEG C by room temperature, constant temperature 150min; Subordinate phase is warming up to 270 DEG C by 180 DEG C, constant temperature 180min; Phase III is warming up to 360 DEG C by 270 DEG C, constant temperature 180min.
Beneficial effect of the present invention is as follows:
Utilize novel process to calcium carbonate modified filling high-performance afterwards cheap and easy to get but expensive tetrafluoroethylene, significantly reduce costs while respective performances being reached.
More unmodified calcium carbonate-filled ptfe composite, significantly promotes elongation at break.
More unmodified calcium carbonate-filled ptfe composite, significantly promotes tensile strength.
Accompanying drawing explanation
Fig. 1: the volume of modified calcium carbonate and unmodified calcium carbonate is on the impact of matrix material tensile strength;
Fig. 2: the volume of modified calcium carbonate and unmodified calcium carbonate is on the impact of fracture of composite materials elongation.
Embodiment
Following examples explain technical scheme of the present invention further, but not as limiting the scope of the invention.
The preparation process of modified calcium carbonate filled polytetrafluoroethylene matrix material of the present invention is as follows:
Calcium carbonate, water, dehydrated alcohol, paraffin mix and blend reflux 90min, cooling, oven dry obtain modified calcium carbonate powder;
Above-mentioned modified calcium carbonate powder and polytetrafluoroethylsuspending suspending powder blended under agitation are obtained compound, compound is put into mold cold pressing formation and obtain composite sheet;
Wrap as in retort furnace with aluminium foil by described composite sheet, program segmenting heats up and sinters: the first stage rises to 180 DEG C by room temperature, constant temperature 150min; Subordinate phase is warming up to 270 DEG C by 180 DEG C, constant temperature 180min; Phase III is warming up to 360 DEG C by 270 DEG C, constant temperature 180min.Obtain modified calcium carbonate filled polytetrafluoroethylene matrix material.
Wherein, raw materials by weight portion meter is as follows:
Wherein, particularly important ground, program segmenting intensification sintering process is as follows:
First stage rises to 180 DEG C by room temperature, constant temperature 150min; Subordinate phase is warming up to 270 DEG C by 180 DEG C, constant temperature 180min; Phase III is warming up to 360 DEG C by 270 DEG C, constant temperature 180min.This program segmenting intensification sintering process of the present invention is that fracture of composite materials elongation and the lifting drawing high intensity have vital role.
Embodiment 1
5g calcium carbonate is added in flask, 50ml deionized water, 0.9ml dehydrated alcohol, 0.05g solid paraffin, 0.004g antioxidant 1010 stirs and is warming up to 92 DEG C, condensing reflux under the condition of oil bath or water-bath, stop stirring after naturally cooling to room temperature, take out solution in flask, dry under 45 DEG C of conditions, obtained modified calcium carbonate powder.
Get the pure polytetrafluoroethylsuspending suspending powder of 95g, blended in high speed agitator with above-mentioned modified calcium carbonate powder, then compound is placed in special die, on vulcanizing press, coldmoulding obtains composite sheet.
The composite sheet suppressed is placed in oven for drying drying for standby; With aluminium foil the composite sheet pressed wrapped and be placed in retort furnace, to heat up sintering with program segmenting: the first stage rises to 180 DEG C by room temperature, constant temperature 150min; Subordinate phase is warming up to 270 DEG C by 180 DEG C, constant temperature 180min; Phase III is warming up to 360 DEG C by 270 DEG C, constant temperature 180min.Obtain 5wt.% modified calcium carbonate filled polytetrafluoroethylene matrix material.
Embodiment 2
10g calcium carbonate is added in flask, 100ml deionized water, 1.8ml dehydrated alcohol, 0.1g solid paraffin, 0.008g antioxidant 1010 stirs and is warming up to 92 DEG C, condensing reflux under the condition of oil bath or water-bath, stop stirring after naturally cooling to room temperature, take out solution in flask, dry under 50 DEG C of conditions, obtained modified calcium carbonate powder.
Get the pure polytetrafluoroethylsuspending suspending powder of 90g, blended in high speed agitator with above-mentioned modified calcium carbonate powder, then compound is placed in special die, on vulcanizing press, coldmoulding obtains composite sheet.
The composite sheet suppressed is placed in oven for drying drying for standby; With aluminium foil the composite sheet pressed wrapped and be placed in retort furnace, to heat up sintering with program segmenting: the first stage rises to 180 DEG C by room temperature, constant temperature 150min; Subordinate phase is warming up to 270 DEG C by 180 DEG C, constant temperature 180min; Phase III is warming up to 360 DEG C by 270 DEG C, constant temperature 180min.Obtain 10wt.% modified calcium carbonate filled polytetrafluoroethylene matrix material.
Embodiment 3
15g calcium carbonate is added in flask, 150ml deionized water, 2.7ml dehydrated alcohol, 0.15g solid paraffin, 0.012g antioxidant 1010 stirs and is warming up to 92 DEG C, condensing reflux under the condition of oil bath or water-bath, stop stirring after naturally cooling to room temperature, take out solution in flask, dry under 55 DEG C of conditions, obtained modified calcium carbonate powder.
Get the pure polytetrafluoroethylsuspending suspending powder of 85g, blended in high speed agitator with above-mentioned modified calcium carbonate powder, then compound is placed in special die, on vulcanizing press, coldmoulding obtains composite sheet.
The composite sheet suppressed is placed in oven for drying drying for standby; With aluminium foil the composite sheet pressed wrapped and be placed in retort furnace, to heat up sintering with program segmenting: the first stage rises to 180 DEG C by room temperature, constant temperature 150min; Subordinate phase is warming up to 270 DEG C by 180 DEG C, constant temperature 180min; Phase III is warming up to 360 DEG C by 270 DEG C, constant temperature 180min.Obtain 15wt.% modified calcium carbonate filled polytetrafluoroethylene matrix material.
The matrix material obtained to embodiment 1,2,3 carries out Elongation test, and contrast with the unmodified calcium carbonate-filled ptfe composite of corresponding proportion, Elongation test adopts High Speed Rail Testing Instruments company limited TCS-2000 tension testing machine, probe temperature 25 DEG C, rate of extension 20mm/min, method for making sample: the CaCO will sintered with the cut-off knife being heated to high temperature
3/ PTFE composite board is cut into dumbbell shaped standard batten.The test result of tensile strength and elongation at break as depicted in figs. 1 and 2.
As can be seen from Figure 1, the fracture of composite materials elongation in embodiment is all better than unmodified matrix material, more unmodified, and modified Materials Fracture elongation all has and significantly promotes.Water and the wet-process modified coated environment provided of ethanol co-mixing system very good, it can make the coated of paraffin evenly, CaCO
3the distribution of particle more disperses, thus improves CaCO
3consistency between powder particle and tetrafluoroethylene, makes microparticle surfaces produce new physics, chemistry, mechanical property and new function, so can significantly promote Materials Fracture elongation.
As can be seen from Figure 2, the matrix material tensile strength in embodiment is all better than unmodified matrix material, more unmodified, and modified tensile strength of material all has and significantly promotes.Water and the wet-process modified coated environment provided of ethanol co-mixing system very good, it can make the coated of paraffin evenly, CaCO
3the distribution of particle more disperses, thus improves CaCO
3consistency between powder particle and tetrafluoroethylene, makes microparticle surfaces produce new physics, chemistry, mechanical property and new function, so can significantly promote Materials Fracture elongation.
Claims (3)
1. the preparation method of modified calcium carbonate filled polytetrafluoroethylene matrix material, is characterized in that comprising the following steps:
By calcium carbonate, water, dehydrated alcohol, paraffin, antioxidant 1010 mix and blend, reflux, cooling, oven dry obtain modified calcium carbonate powder;
Above-mentioned modified calcium carbonate powder and polytetrafluoroethylsuspending suspending powder blended under agitation are obtained compound, compound is put into mold cold pressing formation and obtain composite sheet;
Wrap as in retort furnace with aluminium foil by described composite sheet, program segmenting heats up and sinters, and obtains modified calcium carbonate filled polytetrafluoroethylene matrix material.
2. the preparation method of modified calcium carbonate filled polytetrafluoroethylene matrix material as claimed in claim 1, is characterized in that described raw materials by weight portion meter is as follows:
3. the preparation method of modified calcium carbonate filled polytetrafluoroethylene matrix material as claimed in claim 1, is characterized in that described program segmenting intensification sintering process is as follows:
First stage rises to 180 DEG C by room temperature, constant temperature 150min; Subordinate phase is warming up to 270 DEG C by 180 DEG C, constant temperature 180min; Phase III is warming up to 360 DEG C by 270 DEG C, constant temperature 180min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105623161A (en) * | 2016-04-01 | 2016-06-01 | 武汉工程大学 | Glass fiber/calcium carbonate/polytetrafluoroethylene three-element composite material and preparation method thereof |
| CN106084591A (en) * | 2016-08-05 | 2016-11-09 | 武汉工程大学 | A kind of Gemini surface active modified glass-fiber/calcium carbonate/politef trielement composite material and preparation method thereof |
| CN106221082A (en) * | 2016-07-25 | 2016-12-14 | 武汉工程大学 | A kind of composite of Gemini surface active modified calcium carbonate filled polytetrafluoroethylene and preparation method thereof |
| CN108751874A (en) * | 2018-08-14 | 2018-11-06 | 贵州大兴旺新材料科技有限公司 | A kind of high-performance color pervious asphalt concrete and preparation method thereof |
| CN112029142A (en) * | 2020-08-06 | 2020-12-04 | 武汉工程大学 | Preparation method of oil-absorbing hydrophobic sponge and oil-absorbing hydrophobic sponge prepared by same |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG51634A1 (en) * | 1990-05-11 | 1993-07-15 | Bg Burgaski T Uni | Composition (compound), method for its preparation and application |
| CN102504463A (en) * | 2011-10-18 | 2012-06-20 | 池州市新科建材有限公司 | Modified calcium carbonate and preparation method thereof |
| CN102604282A (en) * | 2012-03-09 | 2012-07-25 | 浙江大学 | Preparing method of PTFE (polytetrafluoroethylene) composite material filled with nano particles |
| CN104530537A (en) * | 2015-01-08 | 2015-04-22 | 大连塑料研究所有限公司 | Manufacturing method and forming device of high-viscosity resin boards |
-
2015
- 2015-08-21 CN CN201510518970.5A patent/CN105061957B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BG51634A1 (en) * | 1990-05-11 | 1993-07-15 | Bg Burgaski T Uni | Composition (compound), method for its preparation and application |
| CN102504463A (en) * | 2011-10-18 | 2012-06-20 | 池州市新科建材有限公司 | Modified calcium carbonate and preparation method thereof |
| CN102604282A (en) * | 2012-03-09 | 2012-07-25 | 浙江大学 | Preparing method of PTFE (polytetrafluoroethylene) composite material filled with nano particles |
| CN104530537A (en) * | 2015-01-08 | 2015-04-22 | 大连塑料研究所有限公司 | Manufacturing method and forming device of high-viscosity resin boards |
Non-Patent Citations (2)
| Title |
|---|
| 唐磊 等: "《轻量化材料技术》", 31 January 2014, 国防工业出版社 * |
| 轻量化材料技术;唐磊 等;《轻量化材料技术》;国防工业出版社;20140131;398 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105623161A (en) * | 2016-04-01 | 2016-06-01 | 武汉工程大学 | Glass fiber/calcium carbonate/polytetrafluoroethylene three-element composite material and preparation method thereof |
| CN106221082A (en) * | 2016-07-25 | 2016-12-14 | 武汉工程大学 | A kind of composite of Gemini surface active modified calcium carbonate filled polytetrafluoroethylene and preparation method thereof |
| CN106084591A (en) * | 2016-08-05 | 2016-11-09 | 武汉工程大学 | A kind of Gemini surface active modified glass-fiber/calcium carbonate/politef trielement composite material and preparation method thereof |
| CN108751874A (en) * | 2018-08-14 | 2018-11-06 | 贵州大兴旺新材料科技有限公司 | A kind of high-performance color pervious asphalt concrete and preparation method thereof |
| CN108751874B (en) * | 2018-08-14 | 2021-08-17 | 贵州大兴旺新材料科技有限公司 | High-performance colored pervious asphalt concrete and preparation method thereof |
| CN112029142A (en) * | 2020-08-06 | 2020-12-04 | 武汉工程大学 | Preparation method of oil-absorbing hydrophobic sponge and oil-absorbing hydrophobic sponge prepared by same |
| CN112029142B (en) * | 2020-08-06 | 2022-08-16 | 武汉工程大学 | Preparation method of oil-absorbing hydrophobic sponge and oil-absorbing hydrophobic sponge prepared by same |
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