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Phosphate side chain-containing polyimide for gasoline desulphurization and preparation method thereof

A polyimide and side chain technology, which is applied in the field of polyimide and its preparation, can solve the problems that the octane number remains unchanged, does not involve changes in the content of aromatic hydrocarbons and octane number, etc. Simple preparation process and high desulfurization efficiency

Inactive Publication Date: 2012-03-07
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN 1686600 reports a method for preparing a blended composite membrane for pergasification gasoline desulfurization, but it does not involve changes in aromatics content and octane number after gasoline desulfurization, and there is no data showing that the octane number remains unchanged after desulfurization

Method used

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  • Phosphate side chain-containing polyimide for gasoline desulphurization and preparation method thereof
  • Phosphate side chain-containing polyimide for gasoline desulphurization and preparation method thereof
  • Phosphate side chain-containing polyimide for gasoline desulphurization and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Under the protection of nitrogen, add 0.05mol of p-hydroxybenzaldehyde, 0.10mol of aniline, and 0.005mol of aniline hydrochloride into the reaction flask. After they are completely dissolved, react at 100°C for 1 hour, cool and precipitate the precipitate, and filter the precipitate to obtain the crude compound , after several times of recrystallization with methanol, evaporated to dryness to obtain pure 4,4-diamino, 4-hydroxytriphenylmethane (ie, compound a of formula 3).

[0045] Under nitrogen protection, dissolve 0.02mol 4,4-diamino,4-hydroxytriphenylmethane in 25ml N,N dimethylacetamide, add 0.02mol pyromellitic dianhydride, stir at room temperature for 3 hours, and then Add 12.5ml xylene solution, heat up to 100°C for dehydration imidization reaction for 5 hours to obtain compound b of formula 8 (wherein R 1 for R 2 for R 3 where n=0 means no hydrocarbon group)

[0046] Dissolve 0.004mol of compound b of formula 8 in 15ml of chloroform under nitrogen protec...

Embodiment 2

[0050] Under the protection of nitrogen, add 0.06mol p-hydroxybenzaldehyde, 0.48mol aniline solution, and 0.042mol aniline hydrochloride into the reaction flask. After they are completely dissolved, react at 150°C for 5 hours, cool and precipitate the precipitate, and filter the precipitate to obtain the crude product The compound was recrystallized several times with methanol, and evaporated to dryness to obtain pure 4,4-diamino, 4-hydroxytriphenylmethane (ie, compound a of formula 3).

[0051] Under nitrogen protection, 0.025mol 4,4'-diamino-4"-hydroxytriphenylmethane was dissolved in 40ml N,N dimethylformamide, and 0.030mol naphthalene tetraic acid dianhydride (ie, the compound of formula 16) was added, Stir at room temperature for 8 hours, then add 20ml of xylene solution, heat up to 130°C for dehydration imidization reaction for 10 hours, to obtain compound b of formula 8 (wherein R 1 for R 2 for R 3 where n=0 means no hydrocarbon group)

[0052] Dissolve 0.005 mol...

Embodiment 3

[0056] Under nitrogen protection, dissolve 0.02mol 3,3'-diamino-4,4'-dihydroxybiphenyl (compound a of formula 6) in 50ml N-methylpyrrolidone, add 0.026mol 3,3', 4,4'-diphenyl ether tetracarboxylic dianhydride (i.e. the compound of formula 18), stirred at room temperature for 8 hours, then added 25ml of xylene solution, raised the temperature to 150°C for dehydration imidization reaction for 12 hours, and obtained the compound of formula 9 Compound b (wherein R 1 for R 2 for R 3 where n=0 means no hydrocarbon group).

[0057] Dissolve 0.01 mol of compound b of formula 9 in 45 ml of dioxane under nitrogen protection, add 0.06 mol of triethylamine and 0.005 mol of cuprous chloride under ice-cooling, and then dropwise dissolve in 40 ml of dioxane within 20 minutes. Diethyl chlorophosphate in the six rings 0.05mol. React at room temperature for 12 hours, reclaim the filtrate, precipitate the polymer in methanol, and obtain the compound c1 of formula 11-1 after vacuum drying...

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Abstract

The invention discloses a phosphate side chain-containing polyimide and a preparation method and application thereof. The phosphate side chain-containing polyimide is prepared by performing condensation polymerization on hydroxyl-containing aromatic diamine monomer and di-anhydride to prepare polyimide and then performing phosphate esterification and hydrolytic synthesis on the polyimide. The phosphate side chain-containing polyimide has a simple preparation process and a low cost, can be made into films used in the process of gasoline desulphurization and has high desulphurization efficiency; after the desulphurization, sulfur residues in gasoline are about 30 ppm; and simultaneously the aromatic hydrocarbon content is reduced by 5 to 10 percent and the octane value is kept unchanged.

Description

technical field [0001] The invention relates to the field of materials, in particular to a polyimide containing phosphoric acid side chains and a preparation method thereof. Background technique [0002] In modern society, automobile exhaust has become the main pollution source of urban atmospheric environment. The sulfur oxides (SO x ), carbon monoxide (CO) and nitrogen oxides (NO x ), which is the main cause of acid rain and seriously pollutes the urban air environment. In order to improve the environmental pollution caused by gasoline combustion, it is necessary to reduce the content of sulfur compounds in gasoline. With the world's increasing emphasis on environmental protection and stricter environmental regulations, the production of low-sulfur and ultra-low-sulfur gasoline is gradually attracting people's attention. There is still a certain gap between my country's national standards for motor gasoline and foreign advanced standards. Since 2005, my country has impl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C10G31/11B01D71/64
Inventor 胡继文卢汝烽
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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