Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of super-cross-linked polymer

A polymer and hyper-crosslinking technology, applied in the chemical field, can solve the problems of uncertain connection sites and connection numbers of crosslinking agents, wide pore size distribution of HCP, and uneven pore size distribution.

Inactive Publication Date: 2019-03-19
EAST CHINA UNIV OF SCI & TECH
View PDF3 Cites 11 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] There are following deficiencies in the preparation method of existing HCP: (1) compared with metal-organic framework (MOF), the pore size distribution of HCP is relatively wide
This is mainly due to the fact that HCP has certain randomness during cross-linking, and the connection sites and number of connections of cross-linking agents are uncertain, resulting in uneven pore size distribution; In the selection stage of the linking agent, there are relatively few studies involving the chemical modification of the building blocks and the cross-linking agent. HCP usually uses anhydrous ferric chloride as a catalyst, and the compound with an aromatic ring is cross-linked with dimethylformal (FDA). united

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of super-cross-linked polymer
  • Preparation method of super-cross-linked polymer
  • Preparation method of super-cross-linked polymer

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0023] The invention provides a preparation method of a hypercrosslinked polymer. Described preparation method comprises the steps:

[0024] Step (a): Add rigid building blocks, rigid cross-linking agents, catalysts and anhydrous solvents into the reaction vessel, and react at 60-90°C for a certain period of time under the protection of an inert gas (such as nitrogen) atmosphere , and then the temperature was raised to 110-130°C to continue the reaction for several hours. Specifically, add rigid building blocks, rigid cross-linking agents, and catalysts into the reaction vessel in sequence, then add anhydrous solvent, and react at a temperature of 60-90°C under the protection of an inert gas (such as nitrogen) atmosphere For some time, then raise the temperature to 110-130°C and continue the reaction for some time.

[0025] The building blocks are modified rigid substances or unmodified rigid substances. Wherein, the rigidity refers to the property that the average position...

Embodiment 1

[0035] A kind of triptycene is the preparation method of the hypercrosslinked polymer of rigid building block and 1,4-p-methoxybenzene as crosslinking agent, comprises the steps:

[0036] (1) Weigh 0.25g (1mmol) triptycene, 1.104g (8mmol) 1,4-p-methoxybenzene, 4.87g (30mmol) anhydrous FeCl 3 Then add 50 mL of anhydrous nitrobenzene to the reaction vessel in turn, and react at 60° C. for 6 hours under the protection of an inert gas (such as nitrogen) atmosphere, then raise the temperature to 110° C. and continue the reaction for 36 hours.

[0037] (2) After the reaction in step (1) is finished, the reaction system is suction filtered, and the crude product is washed repeatedly with dilute hydrochloric acid solution, methylene chloride and methanol solution until the filtrate is colorless.

[0038] (3) Collect the product after washing in step (2), and then further purify by Soxhlet extraction using methanol as a solvent.

[0039] (4) Finally, the product purified in step (3) was...

Embodiment 2

[0043] A kind of nitro-modified triptycene is rigid building block and 1,4-p-methoxybenzene is the preparation method of the hypercrosslinked polymer of crosslinking agent, comprises the steps:

[0044] (1) Nitro-modified triptycene: In a reaction vessel, first add 2.01g (7.9mmol) triptycene to 50mL glacial acetic acid, then slowly add 24mL nitric acid to the above mixture, and react at 70°C After 6 hours, cool to room temperature. Add 100 mL of water to the reaction vessel, stir for 30 minutes, and filter to obtain the crude product. Finally, the white -NO 2 Modified triptycene. to get -NO 2 The modified triptycene was tested by NMR, and the analytical data of the obtained NMR diagram is as follows: 1 H NMR (CDCl 3 ),δ8.22(d,1H),δ7.95(d,1H),δ7.50(d,1H),δ7.40-7.44(m,4H),δ7.03-7.06(m,4H) ,δ5.55(s,1H),δ5.54(s,1H).

[0045] (2) Weigh 0.3g (1mmol) nitro-modified triptycene, 1.035g (7.5mmol) 1,4-p-methoxybenzene, 3.65g (22.5mmol) anhydrous FeCl 3 Then add 30 mL of anhydrous...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a preparation method of a super-cross-linked polymer. The preparation method comprises the following steps: (a) adding a rigid construction unit, a rigid crosslinking agent, a catalyst and an anhydrous solvent into a reaction container, carrying out a reaction for some time at 60-90 DEG C under protection of an N2 or inert gas atmosphere, and then raising the temperature to110-130 DEG C to react for some time continuously; (b) after the reaction in the step (a) is finished, carrying out suction filtration on the reaction system, and washing the filtered coarse product till the filtrate is colorless; (c) collecting and purifying the washed product in the step (b); and (d) drying the purified product in the step (c) to obtain the super-cross-linked polymer.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method for preparing a hypercrosslinked polymer. Background technique [0002] Adsorption separation has the advantages of high separation efficiency and low energy consumption. In recent years, adsorption separation has been used in CO 2 Great progress has been made in capture and storage, large-scale production of pharmaceuticals and fine chemicals. It is estimated that the global demand for adsorbents will reach 11 billion US dollars in 2019. So far, the development of adsorbents has mainly experienced from zeolite molecular sieves, activated carbon, silica, to metal-organic frameworks (MOFs), porous coordination polymerizations (PCPs), purely organic networks of caged molecules, and porous organic polymers ( POP). Currently, although the research of MOFs as solid adsorbents is a hotspot, their thermal and solvent (water) stability issues limit their practical application. Rece...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/02
CPCC08G61/02C08G2261/135C08G2261/1424C08G2261/143C08G2261/314C08G2261/71
Inventor 陈启斌谭慧玲刘洪来
Owner EAST CHINA UNIV OF SCI & TECH