CN106699935B - Manufacture the tetrafluoroethene dispersion resin and preparation method thereof of filter felt staple fiber - Google Patents
Manufacture the tetrafluoroethene dispersion resin and preparation method thereof of filter felt staple fiber Download PDFInfo
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- CN106699935B CN106699935B CN201611255790.3A CN201611255790A CN106699935B CN 106699935 B CN106699935 B CN 106699935B CN 201611255790 A CN201611255790 A CN 201611255790A CN 106699935 B CN106699935 B CN 106699935B
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- dispersion resin
- staple fiber
- tetrafluoroethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/18—Monomers containing fluorine
- C08F114/26—Tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/28—Emulsion polymerisation with the aid of emulsifying agents cationic
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/08—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons
- D01F6/12—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons from polymers of fluorinated hydrocarbons
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- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Filtering Materials (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention relates to polymer resin technology fields, more particularly to a kind of tetrafluoroethene dispersion resin and preparation method thereof for manufacturing filter felt staple fiber, about 60% volume deionized water is added in the preparation method in polymeric kettle, fluorine-containing surfactant is added after evacuation, emulsion stabilizer, pH adjusting agent, initiator, tetrafluoroethylene monomer is then passed to start to react, surfactant is added in reaction process stage by stage, control by stages reaction speed and reaction time, the tetrafluoroethene lotion of the specified molecular weight distribution of acquisition, lotion is deployed using density, cohesion, dehydration and drying, obtain tetrafluoroethene dispersion resin.The features such as tetrafluoroethene dispersion resin obtained by preparation method of the present invention is suitble to manufacture staple fiber with a variety of methods, is made into the filter assemblies such as needled filtering felt, has high dust collection efficiency, and gas concentration of emission is low.
Description
Technical field
The present invention relates to polymer resin technology fields, and in particular to a kind of tetrafluoroethene for manufacturing filter felt staple fiber
Dispersion resin and preparation method thereof.
Background technique
Polytetrafluoroethylene (PTFE) is commonly called as Teflon, is known as " King ", and relative molecular weight reaches millions of or even up to ten million,
Molecular structure is macromolecular linear structure, almost without branch, all C-F keys in macromolecular two sides, and arranged by zigzag fashion,
Since fluorine atom radius is larger, 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 reagents, in addition, polytetrafluoroethylene (PTFE) can be in -196 DEG C -260 DEG C of wider temperature model
Enclose the excellent mechanical property of interior holding；Since the dipole moment of PTFE macromolecular is close to zero, substantially without polarity, therefore insulation performance
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, electric appliance, 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, has had
The standby mature technology that polytetrafluoroethyldispersion dispersion resin production is made into fiber-like textile product, with the weaving such as fiber of its production
Product manufacture into the high-temperature filter material PTFE Nomex as bag-type dusting, and smoke filtration is used under complex working condition, has been shown
Reveal good properties of product and important economic value.
Tetrafluoroethene dispersion resin currently used for staple fiber manufacture is numerous in variety, but production technology is more complex, Yao Tianjia
Various auxiliary agents or modified monomer, and molecular weight distribution is unstable, causes staple fiber processing difficulties and final products performance unstable.
Summary of the invention
The technical problems to be solved by the present invention are: the purpose of the present invention is to provide a kind of systems that molecular weight distribution is stable
Make the tetrafluoroethene dispersion resin and preparation method thereof of filter felt staple fiber.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows: provide a kind of manufacture filter felt short fibre
The tetrafluoroethene dispersion resin preparation method of dimension, includes the following steps:
Step 1: 50~70% volumes of deionized water being added in polymeric kettle, after vacuumizing sky, fluorine-containing surfactants are added
Agent, emulsion stabilizer, pH adjusting agent and initiator, stir evenly, and then pass to pressure in tetrafluoroethylene monomer to polymeric kettle and are
1.8~2.5MPa starts to react, and in reaction, speed of agitator is 40~50r/min, reaction time are as follows: 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 revolving speed is 60~70r/min；Reaction time are as follows:
40min±5min；
Step 3: the fluorine-containing surfactant of remainder 20% being added after step 2, maintenance revolving speed is 60~70r/min, reaction
Time are as follows: 40min ± 5min obtains lotion；
The total reaction time of the step 1 to step 3 is 100min ± 5min, the total addition level of the tetrafluoroethylene monomer
For 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 additional amount of the emulsion stabilizer are 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 lotion deploys using density, cohesion, dehydration and dry, obtains manufacture filter felt with short
The tetrafluoroethene dispersion resin of fiber.
Preferably, described fluorine-containing in the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt staple fiber
Surfactant is perfluorooctanoic acid.
Preferably, in the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt staple fiber, the lotion
Stabilizer is paraffin.
Preferably, in the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt staple fiber, the pH tune
Saving agent is hydrochloric acid or succinic acid.
Preferably, in the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt staple fiber, the initiation
Agent is ammonium persulfate.
Preferably, the tetrafluoroethene dispersion resin preparation method of above-mentioned manufacture filter felt staple fiber specifically includes as follows
Step:
Step 1: deionized water 2500L being added in the polymeric kettle of the 4000L with horizontal spiral blender, vacuumizes, adds
Enter perfluorooctanoic acid 2.4kg, paraffin 80kg, succinic acid 1.2kg and ammonium persulfate 7g, closes inlet and outlet and replaced with nitrogen, analyzed
Oxygen content is less than 20ppm, and reaction kettle is warming up to 80 DEG C, and it is 1.9Mpa that pressure in tetrafluoroethylene monomer to kettle, which is added, with 45r/
The stirring of min speed, starts to react, and reacts 20min；
Step 2: it continuously adds remaining tetrafluoroethylene monomer, improves revolving speed to 65r/min, the reaction was continued 40min；
Step 3: perfluorooctanoic acid 0.6kg being added after step 2, maintenance revolving speed is 60~70r/min, and reaction 40min obtains newborn
Liquid；
Step 4: the tetrafluoroethylene monomer total amount of adding be 800kg, the lotion through density deploy, cohesion, dehydration and
The tetrafluoroethene dispersion resin of manufacture filter felt staple fiber is obtained after drying.
Another technical solution of the invention is to provide a kind of tetrafluoroethene dispersion of above-mentioned manufacture filter felt staple 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 staple fiber tetrafluoroethene dispersion resin and
Preparation method passes through the adding manner of control by stages surfactant in the preparation method reaction process, controls stage by stage
Reaction speed processed and unified reaction time, the tetrafluoroethene cream of specified molecular weight distribution 10,000,000~30,000,000 of acquisition
Liquid, lotion is deployed, agglomerated using density, being dehydrated and drying, obtains the tetrafluoroethene dispersion resin for being suitble to staple fiber manufacture.
Present invention process is simple, stable operation, and without adding special auxiliary agent, high production efficiency, cost is relatively low.Gained tetrafluoro
Ethylene dispersion resin is suitble to manufacture staple fiber with a variety of methods, is made into the filter assemblies such as needled filtering felt, has high dust collection efficiency,
The features such as gas concentration of emission is low has been provided simultaneously with the good characteristics such as tetrafluoroethene heatproof, wear-resisting, corrosion resistant, chemical-resistant stability,
It is widely used in the filtering of the various severe flue gases such as steel, electric power, waste incineration, becomes ideal atmosphere environment protection treating material
Material.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The most critical design 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 more surfactant of first stage addition is reacted, more reaction center is formed at the very start, passes through
After crossing the molecule chain growth of second stage, the phase III adds a small amount of surfactant, is conducive to dispersion stable and efficiently ties
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 manufacturing filter felt staple fiber, includes the following steps:
Step 1: 70% volumes of deionized water being added in polymeric kettle, after vacuumizing sky, fluorine-containing surfactant, cream is added
Liquid stabilizer, pH adjusting agent and initiator, stir evenly, and then passing to pressure in tetrafluoroethylene monomer to polymeric kettle is 2.5MPa
Start to react, in reaction, speed of agitator 50r/min, the reaction time are as follows: 20min；The fluorine-containing surfactant of addition 80%；
Step 2: tetrafluoroethylene monomer is evenly and rapidly passed through after step 1, raising revolving speed is 70r/min；Reaction time are as follows:
40min；
Step 3: the fluorine-containing surfactant of remainder 20% being added after step 2, maintenance revolving speed is 70r/min, reaction time
Are as follows: 40min obtains lotion；
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 cream
The additional amount 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
Answer temperature control at 100 DEG C；
Step 4: step 3 gained lotion deploys using density, cohesion, dehydration and dry, 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 staple fiber of the present invention, by controlling stage by stage
The adding manner of control surface activating agent, control by stages reaction speed and unified reaction time, the specified molecular weight point of acquisition
The tetrafluoroethene lotion of cloth range, lotion is deployed, agglomerated using density, being dehydrated and drying, obtains being suitble to staple fiber manufacture
Tetrafluoroethene dispersion resin.
Embodiment 2
A kind of tetrafluoroethene dispersion resin preparation method manufacturing filter felt staple fiber, includes the following steps:
Step 1: 50% volumes of deionized water being added in polymeric kettle, after vacuumizing sky, fluorine-containing surfactant, cream is added
Liquid stabilizer, pH adjusting agent and initiator, stir evenly, and then passing to pressure in tetrafluoroethylene monomer to polymeric kettle is 1.8MPa
Start to react, in reaction, speed of agitator 40r/min, the reaction time are as follows: 15min；Addition accounts for containing for total addition level quality 80%
Fluorinated 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 revolving speed is 60r/min；Reaction time are as follows: 40min；
Step 3: the fluorine-containing surfactant of remainder 20% being added after step 2, maintenance revolving speed is 60r/min, reaction time
Are as follows: 40min obtains lotion；
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 are the 0.05% of deionized water quality, the cream
The additional amount 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
Answer temperature control at 80 DEG C；
Step 4: step 3 gained lotion deploys using density, cohesion, dehydration and dry, obtains manufacture filter felt with short
The tetrafluoroethene dispersion resin of fiber.
Embodiment 3
A kind of tetrafluoroethene dispersion resin preparation method manufacturing filter felt staple fiber, includes the following steps:
Step 1: deionized water 2500L being added in the polymeric kettle of the 4000L with horizontal spiral blender, vacuumizes, adds
Enter perfluorooctanoic acid 2.4kg, paraffin 80kg, succinic acid 1.2kg and ammonium persulfate 7g, closes inlet and outlet and replaced with nitrogen, analyzed
Oxygen content is less than 20ppm, and reaction kettle is warming up to 80 DEG C, and it is 1.9Mpa that pressure in tetrafluoroethylene monomer to kettle, which is added, with 45r/
The stirring of min speed, starts to react, and reacts 20min；
Step 2: it continuously adds remaining tetrafluoroethylene monomer, improves revolving speed to 65r/min, the reaction was continued 40min；
Step 3: perfluorooctanoic acid 0.6kg being added after step 2, maintenance revolving speed is 60~70r/min, and reaction 40min obtains newborn
Liquid；The reaction pressure of the step 1 to step 3 is controlled in 1.9MPa, and reaction temperature is controlled at 80 DEG C；
Step 4: the tetrafluoroethylene monomer total amount of adding be 800kg, the lotion through density deploy, cohesion, dehydration and
The tetrafluoroethene dispersion resin of manufacture filter felt staple fiber is obtained after drying.
Recirculated cooling water is adjusted in reaction process, control reaction temperature equably increases, and monomer reaction to 800kg stops anti-
It answers.Releasing and obtaining PTFE amount after lotion is agglomerated, dried is 750kg, through examination criteria relative density 2.154, average molecular weight
Suitable for processing PTFE staple fiber between 15,000,000~20,000,000.
Performance such as the following table 1 of the tetrafluoroethene dispersion resin of filter felt staple fiber is made obtained by the above embodiment of the present invention.
Table 1
| Serial 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 |
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (7)
1. a kind of tetrafluoroethene dispersion resin preparation method for manufacturing filter felt staple fiber, which is characterized in that including walking as follows
It is rapid:
Step 1: 50~70% volumes of deionized water being added in polymeric kettle, after vacuumizing, fluorine-containing surfactant, lotion is added
Stabilizer, pH adjusting agent and initiator, stir evenly, then pass in tetrafluoroethylene monomer to polymeric kettle pressure be 1.8~
2.5MPa starts to react, and in reaction, speed of agitator is 40~50r/min, reaction time are as follows: 20min ± 5min；Add Zhan Zongtian
The fluorine-containing surfactant of dosage quality 80%；
Step 2: remaining tetrafluoroethylene monomer is passed through after step 1, raising revolving speed is 60~70r/min；Reaction time are as follows: 40min
±5min；
Step 3: the fluorine-containing surfactant of remainder 20% being added after step 2, maintenance revolving speed is 60~70r/min, reaction time
Are as follows: 40min ± 5min obtains lotion；
The total reaction time of the step 1 to step 3 is 100min ± 5min, and the total addition level of the tetrafluoroethylene monomer is institute
The 30-45% of deionized water quality is stated, the total amount of adding of the fluorine-containing surfactant is the 0.05%- of deionized water quality
1.5%, the additional amount of the emulsion stabilizer is the 2%~4% of deionized water quality, and the step 1 arrives the reaction pressure of step 3
Power control is controlled in 1.8~2.5MPa, reaction temperature at 80~100 DEG C；
Step 4: step 3 gained lotion is deployed, agglomerated using density, being dehydrated and drying, obtains manufacture filter felt staple fiber
Tetrafluoroethene dispersion resin.
2. the tetrafluoroethene dispersion resin preparation method of manufacture filter felt staple fiber according to claim 1, feature
It is, the fluorine-containing surfactant is perfluorooctanoic acid.
3. the tetrafluoroethene dispersion resin preparation method of manufacture filter felt staple fiber according to claim 1, feature
It is, the emulsion stabilizer is paraffin.
4. the tetrafluoroethene dispersion resin preparation method of manufacture filter felt staple fiber according to claim 1, feature
It is, the pH adjusting agent is hydrochloric acid or succinic acid.
5. the tetrafluoroethene dispersion resin preparation method of manufacture filter felt staple fiber according to claim 1, feature
It is, the initiator is ammonium persulfate.
6. the tetrafluoroethene dispersion resin preparation method of manufacture filter felt staple fiber according to claim 1, feature
It is, specifically comprises the following steps:
Step 1: deionized water 2500L being added in the polymeric kettle of the 4000L with horizontal spiral blender, vacuumizes, is added complete
Fluorine ammonium caprylate 2.4kg, paraffin 80kg, succinic acid 1.2kg and ammonium persulfate 7g close inlet and outlet and are replaced with nitrogen, and analysis oxygen contains
Amount is less than 20ppm, and reaction kettle is warming up to 80 DEG C, and it is 1.9Mpa that pressure in tetrafluoroethylene monomer to kettle, which is added, with 45r/min speed
Degree stirring, starts to react, and reacts 20min；
Step 2: it continuously adds remaining tetrafluoroethylene monomer, improves revolving speed to 65r/min, the reaction was continued 40min；
Step 3: perfluorooctanoic acid 0.6kg being added after step 2, maintenance revolving speed is 60~70r/min, and reaction 40min obtains lotion；
Step 4: the tetrafluoroethylene monomer total amount of adding is 800kg, and the lotion is deployed, agglomerated through density, being dehydrated and drying
The tetrafluoroethene dispersion resin of manufacture filter felt staple fiber is obtained afterwards.
7. a kind of tetrafluoroethene dispersion resin preparation method of manufacture filter felt staple fiber described in any one of claims 1-6
The tetrafluoroethene dispersion resin being prepared.
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| CN109702925A (en) * | 2018-12-19 | 2019-05-03 | 福建三农新材料有限责任公司 | A kind of polytetrafluoroethyldispersion dispersion resin drying equipment |
| CN112538125B (en) * | 2020-12-14 | 2022-11-08 | 江西理文化工有限公司 | Preparation method of low molecular weight polytetrafluoroethylene resin |
| CN116217765B (en) * | 2021-12-03 | 2024-04-02 | 中昊晨光化工研究院有限公司 | Polytetrafluoroethylene dispersion resin for dry electrode binder and preparation method thereof |
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| CN103910818A (en) * | 2014-03-21 | 2014-07-09 | 中昊晨光化工研究院有限公司 | Multipurpose polytetrafluoroethylene dispersion resin and preparation method thereof |
| CN104311746A (en) * | 2014-11-17 | 2015-01-28 | 中昊晨光化工研究院有限公司 | Modified teflon preparation method and obtained product thereof |
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| CN103910818A (en) * | 2014-03-21 | 2014-07-09 | 中昊晨光化工研究院有限公司 | Multipurpose polytetrafluoroethylene dispersion resin and preparation method thereof |
| CN104311746A (en) * | 2014-11-17 | 2015-01-28 | 中昊晨光化工研究院有限公司 | Modified teflon preparation method and obtained product thereof |
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Denomination of invention: Tetrafluoroethylene dispersion resin with short fibers for manufacturing filter felt and its preparation method Effective date of registration: 20230925 Granted publication date: 20190326 Pledgee: Industrial and Commercial Bank of China Limited Sanming Sanyuan Branch Pledgor: FUJIAN SANNONG NEW MATERIALS CO.,LTD. Registration number: Y2023980058306 |