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Preparation method for styrenated phenol

A technology for styrenated phenol and styrene, applied in the field of preparation of styrenated phenol, can solve the problems of solid waste pollution, uneven pore distribution, low conversion rate, etc., and achieves pollution reduction, stable reaction process, and corrosion degree. little effect

Inactive Publication Date: 2017-05-10
JIANGSU FEIYA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, it has been suggested that minerals, activated clay, ion exchange resins, and zeolites should be used instead of inorganic acid catalysts to synthesize styrenated phenols. The research on the catalytic effects of ion exchange resins and zeolite catalysts is still in the laboratory development stage, and there is still a heat-resistant Poor, short life, uneven pore distribution, low conversion rate, etc.
Minerals and activated clay have the disadvantages of solid waste pollution and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0012] A preparation method of styrenated phenol, comprising the following steps:

[0013] Step 1: Take phenol and p-toluenesulfonic acid and put them into the container, pass nitrogen gas, and stir fully with the stirring device. The rotation speed of the stirring device is 300-350r / min, heat up to 85°C, and start to add styrene dropwise. The dropping time is less than 2.5 Hour;

[0014] Step 2: After the addition of styrene is completed, the temperature is raised to 120-130°C at a constant speed, and the temperature is kept for 2-2.5 hours;

[0015] Step 3: Stop heating, add triethylamine to the mixture, stir well and then filter, then suction filter and vacuum distill until no liquid evaporates, cool down to below 80°C, and discharge.

[0016] Further, the purity of phenol is greater than 99%, and the purity of styrene is greater than 99%.

[0017] Further, the mass ratio of styrene to phenol is 1.9:1˜2.3:1.

[0018] Further, in step 1, styrene is added dropwise, the dro...

Embodiment 1

[0022] Accurately weigh 200g of phenol and 2.0g of p-toluenesulfonic acid and put them into a dry and clean four-necked flask, fix and install the stirring paddle, and insert thermocouples, spherical condensing reflux tubes and nitrogen gas conduits into the remaining three ports of the four-necked flask. The phenol was melted by heating with nitrogen, and the stirring blade was turned on at a speed of 300 r / min. When the temperature rises to 85°C, 380g of styrene is added dropwise, the dropping rate is controlled to be 2.6g / min, the dropping time does not exceed 2.5h, and the temperature is maintained at 88-92°C. After dropping, the temperature was raised to 120°C at a constant speed, and the heat preservation was started. Stop heating after 2h, add 1.2g triethylamine to neutralize, stir well and filter. Start the vacuum pump, adjust the vacuum degree to 0.095Mpa, and keep the kettle temperature not exceeding 140°C until no liquid evaporates. Cool down to below 80°C and dis...

Embodiment 2

[0024] Accurately weigh 200g of phenol and 4.0g of p-toluenesulfonic acid and put them into a dry and clean four-necked flask, fix and install the stirring paddle, and insert thermocouples, spherical condensing reflux tubes and nitrogen gas conduits into the remaining three ports of the four-necked flask. The phenol was melted by heating with nitrogen, and the stirring paddle was turned on at a speed of 350 r / min. When the temperature rose to 85°C, 460g of styrene was added dropwise, the dropping rate was controlled to be 5g / min, the dropping time was not more than 2.5h, and the temperature was maintained at 92°C. After dropping, the temperature was raised to 120°C at a constant speed, and the heat preservation was started. Stop heating after 2.5h, add 2.4g triethylamine to neutralize, stir well and filter. Start the vacuum pump, adjust the vacuum degree to 0.095Mpa, and keep the kettle temperature not exceeding 140°C until no liquid evaporates. Cool down to below 80°C and d...

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PUM

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Abstract

The invention discloses a preparation method for styrenated phenol. The preparation method comprises the following steps: adding phenol and p-toluenesulfonic acid into a container, introducing nitrogen, carrying out sufficient stirring with a stirring device at a rotating speed of 300 to 350 r / min, carrying out heating to 85 DEG C and then starting addition of styrene drop by drop, wherein the addition lasts for less than 2.5 h; after completion of the addition of styrene, carrying out heating to 120 to 130 DEG C at a constant rate and maintaining the temperature for 2 to 2.5 h; and stopping heating, adding triethylamine into a mixture obtained in the previous step, carrying out full stirring, then successively carrying out filtering, pumping filtration and vacuum distillation until no liquid is distilled off, carrying out cooling to 80 DEG C or below, and then carrying out discharging. According to the invention, the catalyst p-toluenesulfonic acid used in the invention is an organic acid and exerts good promotion effect on the alkylation reaction of phenol with styrene; the acidity of p-toluenesulfonic acid is weaker compared with inorganic strong acids like sulfuric acid and hydrochloric acid, so corrosion to reaction equipment is small; and reaction process is smooth and steady, reaction temperature is easy to control, and prepared styrenated phenol has a shallow color.

Description

technical field [0001] The present disclosure generally relates to the field of antioxidants, specifically to the field of antioxidant production, and in particular to a preparation method of styrenated phenol. Background technique [0002] At present, the traditional styrenated phenol production process in China has problems such as low product yield, low content of secondary substitutes, high cost, and serious equipment corrosion. The catalyst used in the earliest production process is mainly sulfuric acid, which has the advantages of low reaction temperature and fast reaction speed. The disadvantage is that sulfuric acid oxidizes the product and is highly corrosive to equipment. The production process requires post-treatments such as neutralization, filtration, and water washing. The process is cumbersome, the yield is low, and there are three wastes. Later, some enterprises used liquid acid catalysts: hydrochloric acid, oxalic acid, phosphoric acid, polyphosphoric acid,...

Claims

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Application Information

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IPC IPC(8): C07C37/14C07C39/15
CPCC07C37/14C07C39/15
Inventor 曹宏生王宇王忠冬桑凌晨
Owner JIANGSU FEIYA CHEM IND
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