Manufacture tetrafluoroethene dispersion resin of filter felt chopped fiber and preparation method thereof
Technical field
The present invention relates to polymer resin technology field, and in particular to a kind of tetrafluoroethene of manufacture filter felt chopped fiber
Dispersion resin and preparation method thereof.
Background technology
Polytetrafluoroethylene (PTFE) is commonly called as Teflon, is described as " King ", its relative molecular weight reach it is millions of or even up to ten million,
Molecular structure is macromolecular linear structure, almost without side chain, all C-F keys in macromolecular both sides, and arranged by zigzag fashion,
Because fluorine atom radius is larger, so as to form a kind of very stable chemical bond, the carbon atom shielding protection on major key can be risen
Come, strand is difficult to be destroyed.Therefore, PTFE material has good corrosion-resistant, heat resistance and inoxidizability, except melting
Outside alkali metal, hardly corroded by any chemical reagent, additionally, polytetrafluoroethylene (PTFE) can be in -196 DEG C -260 DEG C of wider temperature model
Enclose the excellent mechanical property of interior holding;Because the dipole moment of PTFE macromoleculars is close to zero, substantially without polarity, therefore insulating properties
Very well;The surface free energy of PTFE is low, with height do not adhere to minimum coefficient of friction, also with fabulous noninflammability and
Ageing resistance, these advantages make it in the national economy such as chemical industry, machinery, electronics, electrical equipment, military project, space flight, environmental protection and bridge field
In play the important and pivotal role.
Domestic polytetrafluoroethylene (PTFE) industry has significant progress in recent years, wherein, in fabrics for industrial use industry, have
It is standby that polytetrafluoroethyldispersion dispersion resin is made the maturation process for making fiber-like textile product, weaved with its fiber for producing etc.
Product, manufacture into the high-temperature filter material PTFE Nomexs as bag-type dusting, and smoke filtration is used under complex working condition, have shown
Reveal good properties of product and important economic worth.
Tetrafluoroethene dispersion resin currently used for chopped fiber manufacture is numerous in variety, but production technology is more complicated, to add
Various auxiliary agents or modified monomer, and molecular weight distribution is unstable, causes chopped fiber processing difficulties and final products unstable properties.
The content of the invention
The technical problems to be solved by the invention are:It is an object of the invention to provide a kind of system of molecular weight distribution stabilization
Make tetrafluoroethene dispersion resin of filter felt chopped fiber and preparation method thereof.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is:A kind of manufacture short fibre of filter felt is provided
The tetrafluoroethene dispersion resin preparation method of dimension, comprises the following steps:
Step 1:50~70% volumes of deionized water are added in polymeric kettle, after vacuumizing sky, fluorine-containing surfactants is added
Agent, emulsion stabilizer, pH adjusting agent and initiator, stir, and then pass to pressure in tetrafluoroethylene monomer to polymeric kettle and are
1.8~2.5MPa starts reaction, and in reaction, speed of agitator is 40~50r/min, and the reaction time is:20min±5min;Addition
Account for the fluorine-containing surfactant of total addition level quality 80%;
Step 2:Remaining tetrafluoroethylene monomer is passed through after step 1, raising rotating speed is 60~70r/min;Reaction time is:
40min±5min;
Step 3:Remaining 20% fluorine-containing surfactant is added after step 2, maintenance rotating speed is 60~70r/min, reaction
Time is:40min ± 5min, obtains emulsion;
The total reaction time that the step 1 arrives step 3 is 100min ± 5min, the total addition level of the tetrafluoroethylene monomer
It is the 30-45% of the deionized water quality, the total amount of adding of the fluorine-containing surfactant is deionized water quality
0.05%-1.5%, the addition of the emulsion stabilizer is the 2%~4% of deionized water quality, and the step 1 arrives step 3
Reaction pressure control in 1.8~2.5MPa, reaction temperature is controlled at 80~100 DEG C;
Step 4:Step 3 gained emulsion by density allotment, cohesion, dehydration and is dried again, obtains manufacture filter felt with short
The tetrafluoroethene dispersion resin of fiber.
Preferably, it is described fluorine-containing in the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt chopped fiber
Surfactant is perfluorooctanoic acid.
Preferably, in the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt chopped fiber, the emulsion
Stabilizer is paraffin.
Preferably, in the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt chopped fiber, the pH is adjusted
Section agent is hydrochloric acid or succinic acid.
Preferably, in the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt chopped fiber, the initiation
Agent is ammonium persulfate.
Preferably, the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt chopped fiber specifically includes as follows
Step:
Step 1:Deionized water 2500L is added in the polymeric kettle of the 4000L with horizontal spiral agitator, is vacuumized, plus
Enter perfluorooctanoic acid 2.4kg, paraffin 80kg, succinic acid 1.2kg and ammonium persulfate 7g, close import and export nitrogen displacement, analysis
Oxygen content is less than 20ppm, and reactor is warming up into 80 DEG C, and it is 1.9Mpa to add pressure in tetrafluoroethylene monomer to kettle, with 45r/
Min speed is stirred, and starts reaction, reacts 20min;
Step 2:Remaining tetrafluoroethylene monomer is continuously added, rotating speed to 65r/min is improved, continues to react 40min;
Step 3:Perfluorooctanoic acid 0.6kg is added after step 2, maintenance rotating speed is 60~70r/min, and reaction 40min obtains newborn
Liquid;
Step 4:The tetrafluoroethylene monomer total amount of adding be 800kg, the emulsion through density allocate, cohesion, dehydration and
The tetrafluoroethene dispersion resin of manufacture filter felt chopped fiber is obtained after drying.
Another technical scheme of the invention is to provide a kind of tetrafluoroethene dispersion of above-mentioned manufacture filter felt chopped fiber
The tetrafluoroethene dispersion resin that process for preparing resins is prepared.
The beneficial effects of the present invention are:The present invention relates to manufacture filter felt chopped fiber tetrafluoroethene dispersion resin and
Its preparation method, by the feed postition of control by stages surfactant in the preparation method course of reaction, controls stage by stage
Reaction speed processed and unified reaction time, the tetrafluoroethene breast of specified molecular weight distribution 10,000,000~30,000,000 of acquisition
Liquid, emulsion by density allotment, cohesion, dehydration and is dried again, obtains being adapted to the tetrafluoroethene dispersion resin of chopped fiber manufacture.
Present invention process is simple, stable operation, and without adding special auxiliary agent, production efficiency is high, and cost is relatively low.Gained tetrafluoro
Ethene dispersion resin is adapted to manufacture chopped fiber with various methods, makes the filter assemblies such as needled filtering felt, high with efficiency of dust collection,
The low feature of gas concentration of emission, has been provided simultaneously with the good characteristic such as tetrafluoroethene heatproof, wear-resisting, corrosion resistant, chemical-resistant stability,
The filtering of the various severe flue gases such as steel, electric power, waste incineration is widely used in, as preferable air environment protection treating material
Material.
Specific embodiment
To describe technology contents of the invention, the objects and the effects in detail, it is explained below in conjunction with implementation method.
The design of most critical of the present invention is:The relatively small molecular weight resin that molecular weight is in 10,000,000~30,000,000 needs phase
To efficiently reaction controlling, the reaction first stage adds more surfactant, more reaction center is formed at the very start, passes through
After crossing the strand growth of second stage, the phase III adds a small amount of surfactant, is conducive to dispersion stable efficiently to tie
Shu Juhe, obtains the tetrafluoroethene dispersion liquid of the relatively small narrow distribution of molecular weight.
Embodiment 1
A kind of tetrafluoroethene dispersion resin preparation method for manufacturing filter felt chopped fiber, comprises the following steps:
Step 1:70% volumes of deionized water is added in polymeric kettle, after vacuumizing sky, fluorine-containing surfactant, breast is added
Liquid stabilizer, pH adjusting agent and initiator, stir, and it is 2.5MPa to then pass to pressure in tetrafluoroethylene monomer to polymeric kettle
Start reaction, in reaction, speed of agitator is 50r/min, the reaction time is:20min;The fluorine-containing surfactant of addition 80%;
Step 2:Tetrafluoroethylene monomer is evenly and rapidly passed through after step 1, raising rotating speed is 70r/min;Reaction time is:
40min;
Step 3:Remaining 20% fluorine-containing surfactant is added after step 2, maintenance rotating speed is 70r/min, reaction time
For:40min, obtains emulsion;
The total reaction time of the step 1 to step 3 is 100 minutes, and the total addition level of the tetrafluoroethylene monomer is institute
The 48% of deionized water quality is stated, the total amount of adding of the fluorine-containing surfactant is the 1.5% of deionized water quality, the breast
The addition of liquid stabilizer is the 4% of deionized water quality, and the reaction pressure of the step 1 to step 3 is controlled in 2.5MPa, instead
Temperature control is answered at 100 DEG C;
Step 4:Step 3 gained emulsion by density allotment, cohesion, dehydration and is dried again, obtains manufacture filter felt with short
The tetrafluoroethene dispersion resin of fiber.
In the tetrafluoroethene dispersion resin preparation method of the above-mentioned manufacture filter felt chopped fiber of the present invention, by controlling stage by stage
The feed postition of control surface activating agent, control by stages reaction speed and unified reaction time, the specified molecular weight point of acquisition
The tetrafluoroethene emulsion of cloth scope, emulsion by density allotment, cohesion, dehydration and is dried again, obtains being adapted to chopped fiber manufacture
Tetrafluoroethene dispersion resin.
Embodiment 2
A kind of tetrafluoroethene dispersion resin preparation method for manufacturing filter felt chopped fiber, comprises the following steps:
Step 1:50% volumes of deionized water is added in polymeric kettle, after vacuumizing sky, fluorine-containing surfactant, breast is added
Liquid stabilizer, pH adjusting agent and initiator, stir, and it is 1.8MPa to then pass to pressure in tetrafluoroethylene monomer to polymeric kettle
Start reaction, in reaction, speed of agitator is 40r/min, the reaction time is:15min;Addition accounts for containing for total addition level quality 80%
Fluorine surfactant;
The fluorine-containing surfactant, emulsion stabilizer, pH adjusting agent and initiator are respectively perfluorooctanoic acid, paraffin,
Succinic acid, ammonium persulfate.
Step 2:Remaining tetrafluoroethylene monomer is passed through after step 1, raising rotating speed is 60r/min;Reaction time is:40min;
Step 3:Remaining 20% fluorine-containing surfactant is added after step 2, maintenance rotating speed is 60r/min, reaction time
For:40min, obtains emulsion;
The total reaction time of the step 1 to step 3 is 95min, and the total addition level of the tetrafluoroethylene monomer is described
The 30% of deionized water quality, the total amount of adding of the fluorine-containing surfactant is the 0.05% of deionized water quality, the breast
The addition of liquid stabilizer is the 2% of deionized water quality, and the reaction pressure of the step 1 to step 3 is controlled in 1.8MPa, instead
Temperature control is answered at 80 DEG C;
Step 4:Step 3 gained emulsion by density allotment, cohesion, dehydration and is dried again, obtains manufacture filter felt with short
The tetrafluoroethene dispersion resin of fiber.
Embodiment 3
A kind of tetrafluoroethene dispersion resin preparation method for manufacturing filter felt chopped fiber, comprises the following steps:
Step 1:Deionized water 2500L is added in the polymeric kettle of the 4000L with horizontal spiral agitator, is vacuumized, plus
Enter perfluorooctanoic acid 2.4kg, paraffin 80kg, succinic acid 1.2kg and ammonium persulfate 7g, close import and export nitrogen displacement, analysis
Oxygen content is less than 20ppm, and reactor is warming up into 80 DEG C, and it is 1.9Mpa to add pressure in tetrafluoroethylene monomer to kettle, with 45r/
Min speed is stirred, and starts reaction, reacts 20min;
Step 2:Remaining tetrafluoroethylene monomer is continuously added, rotating speed to 65r/min is improved, continues to react 40min;
Step 3:Perfluorooctanoic acid 0.6kg is added after step 2, maintenance rotating speed is 60~70r/min, and reaction 40min obtains newborn
Liquid;The step 1 is controlled in 1.9MPa to the reaction pressure of step 3, and reaction temperature is controlled at 80 DEG C;
Step 4:The tetrafluoroethylene monomer total amount of adding be 800kg, the emulsion through density allocate, cohesion, dehydration and
The tetrafluoroethene dispersion resin of manufacture filter felt chopped fiber is obtained after drying.
Recirculated cooling water is adjusted in course of reaction, controlling reaction temperature is equably raised, monomer reaction to 800kg stops anti-
Should.It is 750kg to release emulsion and PTFE amounts are obtained after cohesion, drying, after testing standard relative density 2.154, mean molecule quantity
It is suitable for processing PTFE chopped fibers between 15,000,000~20,000,000.
The above embodiment of the present invention gained makes the performance such as table 1 below of the tetrafluoroethene dispersion resin of filter felt chopped fiber.
Table 1
Sequence number |
Project |
Index |
1 |
Cleannes |
Plate face is clean, homogeneous |
2 |
Tensile strength (MPa) |
31.5 |
3 |
Elongation at break (%) |
330 |
4 |
Bulk density (g/L) |
490 |
5 |
Average grain diameter (um) |
520 |
6 |
Moisture content (%) |
0.035 |
7 |
Fusing point (DEG C) |
328 |
8 |
Standard relative density |
2.165 |
9 |
Thermal instability |
30 |
10 |
Extrusion pressure (MPa) |
80 |
Embodiments of the invention are the foregoing is only, the scope of the claims of the invention is not thereby limited, it is every to utilize this hair
The equivalents that bright description is made, or the technical field of correlation is directly or indirectly used in, similarly it is included in this hair
In bright scope of patent protection.