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Fluoropolymer microsphere

一种聚合物、微球的技术，应用在运输和包装、涂层、薄料处理等方向，能够解决反应压力高、反应过程制约二氧化碳流体等问题，达到保证稳定性、降低压力、缩短时间的效果

Inactive Publication Date: 2013-06-05
SHANGHAI WEIKAI CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the traditional polymerization reaction needs to be carried out under heating conditions (for example, above 50°C), and the reaction temperature is higher than the critical temperature of carbon dioxide (31.3°C). Therefore, carbon dioxide must be in a supercritical state, and correspondingly, the reaction pressure usually needs to be higher. (≥200bar), the expensive equipment cost and slow reaction process restrict the practical application of carbon dioxide fluid in the preparation of microspheres

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] This example describes a synthetic example of the stabilizing dispersant employed in this invention. Azobisisobutyronitrile (AIBN) thermal initiator (0.04g, 0.00025mol), BPTTC (0.24g, 0.0010mol) and two polymerized monomers in different proportions (15.3g in total, see Table 1 for the charging ratio) were dissolved In 10 ml of trifluorotoluene, under nitrogen atmosphere, heated to 60 °C, and random copolymerization was carried out for 48 hours. The polymer was precipitated from solution with methanol and filtered and dried in a vacuum oven at 45°C for 24 hours.

[0041] Table 1 Monomer composition ratio and number average molecular weight of random copolymers (M n )

[0042]

[0043]

[0044] In Table 1, in the second monomer, BA refers to butyl acrylate, DMAEMA refers to dimethylaminoethyl methacrylate; the first monomer is dodecafluoroheptyl methacrylate (HFPMA); the monomer charging ratio refers to is the weight ratio of the first monomer and the second mono...

Embodiment 2

[0047] The fluoropolymer microspheres of this example were prepared by the following steps: photoinitiated dispersion polymerization in a 40ml autoclave (such as figure 1 shown), the quartz glass above the autoclave was used as the light transmission window, and a 3W LED (wavelength range: 405-410 nm) was used as the light source. The reactor was placed in an ice-water bath with a magnetic stirrer below. The polymerized monomer isobornyl acrylate (IBOA), the photoinitiator 2,4,6-trimethylbenzoyldiphenylphosphine oxide (TPO) and the stabilized dispersant S-DM-1 were added to the reactor respectively. . The concentration of the polymerized monomer IBOA in the total volume of the polymerized monomer and liquid carbon dioxide is 0.10g / ml, the amount of the photoinitiator TPO is 2.0wt% of the polymerized monomer, and the amount of the stabilized dispersant S-DM-1 is the polymerized monomer. 7wt% of the body. A small amount of carbon dioxide gas was introduced, and then slowly di...

Embodiment 3

[0051] In this example, the stable dispersant S-DM-2 is used instead of S-DM-1 in the example, and the types and amounts of other reagents and the implementation process are the same as those in Example 2. Scanning Electron Microscopy (SEM) of the resulting product is shown in figure 2 ,Depend on figure 2 It can be seen that the obtained polymer product is a regular spherical shape, there is no obvious adhesion between the microspheres, and the particle size of the microspheres is basically 1-10 microns, which is suitable as an additive for coating products.

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Abstract

The invention discloses a fluoropolymer microsphere. Polymerizable monomer, photoinitiator and a stable dispersion agent are added into a reaction kettle, carbon dioxide gas is injected to empty the reaction kettle; liquid carbon dioxide is injected, the kettle is irradiated by an initiating light source after the temperature and the pressure of the kettle are stable, and the carbon dioxide reacts at the temperature below 20 DEGC to 30 DEG C and 20 bar to 70 bar. The polymerizable monomer accounts for 0.02g-2g / ml of the concentration of the total volume of the reactant, and the weight ratio among the photoinitiator, the stable dispersion agent and the polymerizable is (0.3-1.0) : (2-20) : 100. After reaction is ended up, the temperature recovers to an indoor temperature, sediment are washed by the liquid carbon dioxide so that the fluoropolymer microsphere can be obtained. The fluoropolymer microsphere which covers the surface of the microsphere can reduce the surface energy of the microsphere, and is beneficial to migration of the microsphere to the coating surface. Tertiary amine group which leads to the fluoropolymer enables the microsphere to be fixedly bonded to a cross-linked network, and is beneficial to closely bonding of the microsphere and the coating. Introduction of reversible addition fragmentation chain (RAFT) active group enables the microsphere to be firmly anchored on the coating firm so that the stability of the coating is solidified.

Description

technical field [0001] The invention relates to the field of synthesis of polymer microspheres, in particular to a fluorine-containing polymer microsphere. Background technique [0002] Polymer microspheres refer to polymer materials or polymer composite materials with diameters ranging from nanometers to micrometers and spherical or nearly spherical geometric shapes. Polymer microspheres have long had special and important applications in the fields of electronic information, biomedical technology and coatings due to their special size and structure. [0003] In coatings, in addition to improving coating properties (mechanical properties, electromagnetic properties, etc.), microspheres can also be used to adjust coating surface properties, such as optical properties such as extinction and light diffusion, as well as abrasion resistance and scratch resistance. , weather resistance, etc. In the application of high-solid content photocurable coatings, due to the rapid curing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F2/48C08F2/04C09D7/12
CPCC08F293/00C09D7/12C08F2/48C08F293/005C08F2438/03C08F220/24C09D7/40Y10T428/2982C09D7/65C08F265/06
Inventor 虞明东袁慧雅
Owner SHANGHAI WEIKAI CHEM
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