CN109721670A - A kind of preparation method of narrow partial size suspension injecting tetrafluoroethylene PTFE resin - Google Patents
A kind of preparation method of narrow partial size suspension injecting tetrafluoroethylene PTFE resin Download PDFInfo
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- CN109721670A CN109721670A CN201811335958.0A CN201811335958A CN109721670A CN 109721670 A CN109721670 A CN 109721670A CN 201811335958 A CN201811335958 A CN 201811335958A CN 109721670 A CN109721670 A CN 109721670A
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Abstract
The present invention discloses a kind of preparation method of narrow partial size suspension injecting tetrafluoroethylene (PTFE) resin, 1, tetrafluoroethene be polymerized monomer, through ingredient, polymerization, suspension polytetrafluoroethylene resin is made；2, when deionized water is 100 parts, di-tert-butyl peroxide is 1.14 × 10‑2Part, ferrous naphthenate is 2.28 × 10‑2Part, perfluoro-cyclicether is 2.28 × 10‑1Part；3, polymerization initiation temperature is 40 DEG C, 40~60 DEG C are maintained in polymerization process, reaction kettle is at the uniform velocity added in 90 minutes in the form of mass percent concentration is 1% weak solution in a definite value of the reaction pressure between 1.6~3.0MPa of gauge pressure, constant pressure reaction, ferrous naphthenate；4, step 3 resulting material is washed repeatedly more than three times with deionized water, until the filtrate conductivity measured is down to 1 μ S/m or less；Finally with not higher than 200 DEG C temperature drying.
Description
Technical field
The present invention relates to a kind of preparation methods of narrow partial size suspension injecting tetrafluoroethylene PTFE resin, belong to fluoro-containing plastic and its system
Preparation Method technical field.
Background technique
The difference of suspension tetrafluoro resin quality is the particle size by them, particle diameter distribution and particle shape difference institute
It causes, therefore particle size distribution range is narrower, stronger using specific aim, the probability for " defect point " occur is lower, the processing of product
Performance and product properties are better.
In common initiators for polymerization, inorganic peroxide (such as ammonium persulfate) is at low cost and without special molten
Agent, but inorganic peroxide belongs to water soluble starter, and the tetrafluoroethylene monomer being dissolved in the water on a small quantity can be made to aggregate into molecule
Amount and partial size are far below " impurity " of major constituent；Perfluor organic peroxide (such as perfluoroacyl peroxides) advantage is nothing
It need to make the processing of molecule tail end base, disadvantage is that spontaneous thermal phenomenon can occur in the course of the polymerization process, makes to exceed in kettle temperature certain time
Control range, reaction speed generate deviation, influence molecular weight and particle diameter distribution.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of narrow partial size suspension injecting tetrafluoroethylene PTFE resin, are mainly
Selfdecomposition present in solution organic initiators polymerization reaction overruns and leads to molecular weight and the widened technology of particle size distribution range
Problem.
In order to achieve the above object, the technical solution adopted is that: use a kind of narrow partial size suspension injecting tetrafluoroethylene PTFE tree
The preparation method of rouge, it is characterised in that step are as follows:
Step 1, using deionized water as medium, di-tert-butyl peroxide is initiator, and ferrous naphthenate is reducing agent, perfluor
Cyclic ethers is buffer solvent, and tetrafluoroethene is polymerized monomer, and through ingredient, polymerization, suspension polytetrafluoroethylene resin is made；
Step 2, on the basis of the additional amount of deionized water based on weight part, when deionized water is 100 parts, di-t-butyl peroxide
Compound is 1.14 × 10-2Part, ferrous naphthenate is 2.28 × 10-2Part, perfluoro-cyclicether is 2.28 × 10-1Part.；
Step 3, polymerization initiation temperature are 40 DEG C, are maintained at 40~60 DEG C in polymerization process, reaction pressure be gauge pressure 1.6~
A definite value between 3.0MPa, constant pressure reaction, ferrous naphthenate is in the form of mass percent concentration is 1% weak solution 90
Reaction kettle is at the uniform velocity added in minute；
Step 4, step 3 resulting material are washed repeatedly more than three times with deionized water, until the filtrate conductivity measured is down to 1
μ S/m or less；Finally with not higher than 200 DEG C temperature drying, the suspending resin of solid powder state is obtained.
It can be with the beneficial effects of the present invention are: using oxidation-reduction trigger system and reducing agent whole process constant speed being allowed to be added
Keep reaction rate more stable, perfluor buffer solvent can make more labile initiator be not easy to divide certainly before acting on reducing agent
Solution, and the fluorination sealing end of tail end base can be completed while polymerization, molecular weight of product and partial size are more accurate, and distribution narrows.
The object of the present invention is to provide a kind of preparation methods of narrow partial size suspension injecting tetrafluoroethylene (PTFE) resin, primarily to solving
Selfdecomposition present in organic initiators polymerization reaction is overrun the technical issues of causing molecular weight and particle size distribution range to expand, and is belonged to
Fluoro-containing plastic and preparation method thereof technical field.It is characterized in that di-tert-butyl peroxide is to draw using deionized water as medium
Agent is sent out, ferrous naphthenate is reducing agent, and perfluoro-cyclicether is buffer solvent, and tetrafluoroethene is polymerized monomer, constant pressure reaction, reduction
Reaction kettle is added in agent full stroke uniform.The beneficial effects of the present invention are: using oxidation-reduction trigger system and making reducing agent whole
Constant speed addition can make reaction rate more stable, and perfluor buffer solvent can make more labile initiator act on it with reducing agent
Before be not easy selfdecomposition, and the fluorination sealing end of tail end base can be completed while polymerization, molecular weight of product and partial size are more accurate, distribution
Range narrows.
Specific embodiment
Below by embodiment, technical solution of the present invention is described further, it is intended to make ordinary skill people
Member is it will be appreciated that and implement of the invention.It should be noted that being based on this hair the present invention is not limited to revealed most preferred embodiment
Bright enlightenment, any obvious transformation or equivalent substitute, it should also be considered within protection scope of the present invention.
Embodiment 1:
(1) it is that 65L water is added in 100L reaction kettle in volume, makees evacuation replacement Treatment, temperature is controlled at 40 DEG C, then by tetrafluoro
Reaction kettle is added in ethylene, and pressure is adjusted to 2.0MPa and whole maintenance.
(2) 7.4g di-tert-butyl peroxide, 148g perfluoro-cyclicether are mixed with mulser；
(3) it is added in step (1) reaction kettle with the liquid that metering pump prepares step (2)；
(4) the ferrous naphthenate solution that 1.48L mass percent concentration is 1% is continued into step (1) reaction kettle with metering pump
It is added；
(5) reaction is terminated after the completion of cycloalkanes ferrous iron solution is added；
The present embodiment measures, partial size D50=240, D90=310, D90/D50=1.3
Embodiment 2:
Reactor pressure described in step (1) in embodiment 1 is changed to 3.0MPa, the other the same as in Example 1 operation.
The present embodiment measures, partial size D50=270, D90=325, D90/D50=1.2
Embodiment 3:
Reactor volume described in step (1) in embodiment 1 is changed to 10L, water is changed to 5.5L, two uncles described in step (2)
Butylperoxide is changed to 0.7g, and perfluoro-cyclicether is changed to 15g, and ferrous naphthenate described in step (4) is changed to 100ml, Qi Tatong
Embodiment 1 operates.
The present embodiment measures, partial size D50=280, D90=406, D90/D50=1.45
Embodiment 4:
Reactor pressure described in step (1) in embodiment 1 is changed to 2.0MPa, the other the same as in Example 1 operation.
The present embodiment measures, partial size D50=210, D90=271, D90/D50=1.29
The particle size data that powder commodity most often indicate is exactly D50 and D90, and D90 represents the maximum particle diameter of 90% particle, and D50 is represented
The maximum particle diameter of 50% particle, the two is closer, illustrates that particle diameter distribution is narrower, data that we find and with existing production
Product suspension made from technique is through detecting, and D90/D50 is substantially 2 or so, therefore the detection data of above-described embodiment can be tested
Demonstrate,prove implementation result of the invention.
Claims (1)
1. a kind of preparation method of narrow partial size suspension injecting tetrafluoroethylene PTFE resin, it is characterised in that step are as follows:
Step 1, using deionized water as medium, di-tert-butyl peroxide is initiator, and ferrous naphthenate is reducing agent, perfluor
Cyclic ethers is buffer solvent, and tetrafluoroethene is polymerized monomer, and through ingredient, polymerization, suspension polytetrafluoroethylene resin is made；
Step 2, on the basis of the additional amount of deionized water based on weight part, when deionized water is 100 parts, di-t-butyl peroxide
Compound is 1.14 × 10-2Part, ferrous naphthenate is 2.28 × 10-2Part, perfluoro-cyclicether is 2.28 × 10-1Part；
Step 3, polymerization initiation temperature are 40 DEG C, are maintained at 40~60 DEG C in polymerization process, reaction pressure be gauge pressure 1.6~
A definite value between 3.0MPa, constant pressure reaction, ferrous naphthenate is in the form of mass percent concentration is 1% weak solution 90
Reaction kettle is at the uniform velocity added in minute；
Step 4, step 3 resulting material are washed repeatedly more than three times with deionized water, until the filtrate conductivity measured is down to 1
μ S/m or less；Finally with not higher than 200 DEG C temperature drying, the suspending resin of solid powder state is obtained.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811335958.0A CN109721670A (en) | 2018-11-12 | 2018-11-12 | A kind of preparation method of narrow partial size suspension injecting tetrafluoroethylene PTFE resin |
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| CN201811335958.0A CN109721670A (en) | 2018-11-12 | 2018-11-12 | A kind of preparation method of narrow partial size suspension injecting tetrafluoroethylene PTFE resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818823A (en) * | 2019-11-06 | 2020-02-21 | 江西理文化工有限公司 | Preparation method of tetrafluoroethylene homopolymerization resin by ultrahigh molecular weight suspension method |
| CN114957520A (en) * | 2022-05-09 | 2022-08-30 | 江苏梅兰化工有限公司 | Preparation method of suspended PTFE resin spherical medium particle molding material |
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| JP3005325B2 (en) * | 1990-07-13 | 2000-01-31 | デュネオン・ゲーエムベーハー | Preparation of tetrafluoroethylene polymer in aqueous suspension |
| CN101113189A (en) * | 2007-08-24 | 2008-01-30 | 山东东岳高分子材料有限公司 | Method for preparing modified polytetrafluoroethylene |
| CN102964503A (en) * | 2012-11-16 | 2013-03-13 | 中昊晨光化工研究院有限公司 | Preparation method of modified polytetrafluoroethylene suspension resin |
| CN107778396A (en) * | 2016-08-24 | 2018-03-09 | 中昊晨光化工研究院有限公司 | A kind of polytetrafluoroethylsuspending suspending resin and preparation method thereof |
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- 2018-11-12 CN CN201811335958.0A patent/CN109721670A/en active Pending
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| JP3005325B2 (en) * | 1990-07-13 | 2000-01-31 | デュネオン・ゲーエムベーハー | Preparation of tetrafluoroethylene polymer in aqueous suspension |
| CN101113189A (en) * | 2007-08-24 | 2008-01-30 | 山东东岳高分子材料有限公司 | Method for preparing modified polytetrafluoroethylene |
| CN102964503A (en) * | 2012-11-16 | 2013-03-13 | 中昊晨光化工研究院有限公司 | Preparation method of modified polytetrafluoroethylene suspension resin |
| CN107778396A (en) * | 2016-08-24 | 2018-03-09 | 中昊晨光化工研究院有限公司 | A kind of polytetrafluoroethylsuspending suspending resin and preparation method thereof |
Non-Patent Citations (1)
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| 孙酣经等: "《化工新材料产品及应用手册》", 31 January 2002, 北京：中国石化出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818823A (en) * | 2019-11-06 | 2020-02-21 | 江西理文化工有限公司 | Preparation method of tetrafluoroethylene homopolymerization resin by ultrahigh molecular weight suspension method |
| CN114957520A (en) * | 2022-05-09 | 2022-08-30 | 江苏梅兰化工有限公司 | Preparation method of suspended PTFE resin spherical medium particle molding material |
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