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Method for synthesizing industrial auxiliary N-butylphthalimide

A technology of n-butyl phthalimide and phthalimide, applied in the direction of organic chemistry and the like, can solve the problems of harsh reaction conditions, high price, and the production cost cannot meet the needs of large-scale use, and achieves zero emission, Avoid the effect of high temperature reaction

Active Publication Date: 2014-07-16
安徽翰邦科技咨询有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthetic route using phthalic anhydride and n-butylamine as substrates requires high-temperature reaction, and the reaction conditions are harsh; in the synthetic route using phthalimide potassium salt and halogenated n-butane as reaction substrates, the two substrates are expensive , the production cost cannot satisfy the final product and it is used in large quantities as cheap industrial additives

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 100g of phthalimide (0.68mol) and 800ml of absolute ethanol into a 2000ml four-necked flask equipped with an electromagnetic stirrer, a reflux condenser and a thermometer, and add dropwise 480ml of 80gKOH / L methanol solution (0.69 mol). After the dropwise addition was completed, the mixture was stirred overnight at room temperature. After filtering, the filter cake was rinsed with fresh methanol and then dried to obtain 110 g of potassium phthalimide. Prepare a 2% acetonitrile solution with the prepared potassium phthalimide for later use.

[0043] In the airtight and light-proof fume hood, add 14.7 phthalimide (0.1mol) and 300ml acetonitrile in the 1000ml four-neck flask equipped with electromagnetic stirrer, reflux condenser and thermometer, after stirring and dissolving until clear and transparent, The acetonitrile solution of the potassium phthalimide salt was added dropwise until the pH was 7.5-8.0. 12 g of 1-butene (0.21 mol) were introduced with stirri...

Embodiment 2

[0047] In the airtight and light-proof fume hood, add 14.7 phthalimide (0.1mol) and 1000ml acetonitrile in the 2000ml four-necked flask equipped with electromagnetic stirrer, reflux condenser, tail gas discharge pipe and thermometer, stir and dissolve to After being clear and transparent, add the acetonitrile solution of the above potassium phthalimide salt dropwise until the pH is 7.5-8.0. 28 g of 1-butene (0.5 mol) were introduced with stirring. Turn on the ultraviolet lamp for irradiation, slowly heat up the water bath to 50° C., and keep stirring at this temperature for 10 hours.

[0048] After the reaction was completed, the water bath heating was removed, and the post-treatment operation according to Example 1 obtained 17.3 g of a light yellow viscous liquid, with a yield of 85.22%. The gas chromatography analysis content is 98.76%.

[0049]

Embodiment 3

[0051] Add 14.7 phthalimide (0.1mol), 200ml acetonitrile, 2.42g benzoyl peroxide (0.01mol) and 300g pre-passed mass fraction in a 1L stainless steel autoclave equipped with an electromagnetic stirrer It is 11.3% 1-butene acetonitrile solution (0.61mol). After airtight, it is heated to 80°C. At this time, the internal pressure of the kettle is 1.7Mpa. Keep the temperature between 80°C and 85°C for two hours, and the maximum gauge pressure in the kettle is 2.1Mpa. Cool to room temperature after the heat preservation is over, open the reaction kettle, and pour out the reaction solution. Acetonitrile was distilled off under reduced pressure. Add 5ml of N,N'-dimethylformamide and 20ml of methanol to the residue, and heat to 50°C to dissolve. Cool to -5°C in an ice-salt bath with stirring, and a white needle-like solid precipitates. Filter quickly, rinse the filter cake with cold petroleum ether, and dry it at 20°C to obtain 4.5 g of white needle crystals. The melting point is 3...

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Abstract

The invention discloses a method for synthesizing an industrial auxiliary N-butylphthalimide. The method comprises the following steps: performing a free radical addition reaction on phthalimide and 1-butene serving as main reacting substrates under an initiator or optical initiation condition to obtain the N-butylphthalimide, wherein the molar ratio of phthalimide to 1-butene in the reacting substrates is 1:1-1:7; the initiator is organic peroxide or inorganic peroxide; the molar ratio of phthalimide to organic peroxide initiator is 5:1-10:1; the molar ratio of phthalimide to inorganic peroxide initiator is 1:1-1:4; the reacting temperature is between normal temperature and 100 DEG C, and the reacting time is 3-24 hours. The method adopts the phthalimide and the 1-butene as raw materials which are low in price and easily available, and has the advantages of mild reacting condition and low production cost.

Description

technical field [0001] The invention relates to a synthesis method of a novel industrial auxiliary agent N-n-butylphthalimide. Background technique [0002] N-n-butylphthalimide, molecular structure formula is: [0003] . [0004] N-n-butyl phthalimide is mainly used as industrial additives in textile, printing and dyeing, cosmetics, ink and other industrial fields. Domestic and foreign commodities are BPI. N-butylphthalimide (BPI) is a non-toxic and environmentally friendly industrial additive approved by EU REACH. Widely used in textile, printing and dyeing, cosmetics, ink and other industrial fields. N-n-butylphthalimide is used as a carrier of disperse dyes in the printing and dyeing industry. It has the advantages of being non-toxic, improving the production environment, and simplifying the dyeing process. Therefore, it is widely used in various fabrics such as polyester, spandex, acrylic fiber, and cotton. in the dyeing process. It can solubilize and assist mos...

Claims

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Application Information

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IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 邹从伟周芬戴久坤沈永刚邹从欢
Owner 安徽翰邦科技咨询有限公司
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