Method of synthesizing high purity 1,3:2,4-di (3,4-dimethyl) benzyl cross sorbic alcohol

A technology of benzylidene sorbitol and dimethyl, which is applied in the field of high purity 1, can solve the problems of coke cleaning trouble, large equipment investment, complex equipment structure, etc., and achieves the effect of simple operation, simple equipment structure and improved reaction yield

Active Publication Date: 2010-05-05
BC P INC CHINA NAT PETROLEUM CORP +1
View PDF5 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the existing technology emphasizes high-speed stirring and strong shearing effects, resulting in complex equipment structure, large equipment investment, and troublesome coke cleaning.

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
  • Method of synthesizing high purity 1,3:2,4-di (3,4-dimethyl) benzyl cross sorbic alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 1L reactor equipped with a condenser and an oil-water separator paddle stirrer, add 18 g of 98% sorbitol, 1.5 g of p-toluenesulfonic acid, 3.0 g of tetrabutylammonium bromide, and cyclohexyl Alkane 315ml, then start the stirrer, and add 29g of 95% 3,4-dimethylbenzaldehyde, and heat to a temperature of 80°C, at which point the cyclohexane refluxes and starts to react. The water generated by the reaction is distilled out together with the cyclohexane, condensed by the condenser, separated by the oil-water separator, the solvent cyclohexane is refluxed into the reaction kettle, and the stirring speed is controlled at about 80 rpm. After reacting for 1 hour, when the reaction system gradually becomes viscous, increase the stirring speed to 100-130 rpm. Then slowly add reaction accelerator methanol solution 160ml at a time, after that, the temperature of the reaction system will gradually decrease, and the viscous state of the material will be alleviated. Keep the refl...

Embodiment 2

[0022] In the 1L reaction kettle that condenser, oil-water separator paddle type stirrer are housed, add content successively and be sorbitol 18g of 98%, p-toluenesulfonic acid 1.5g, tetrabutylammonium chloride 3.0g, 315ml of cyclohexane, then start the stirrer, and add 29g of 3,4-dimethylbenzaldehyde whose content is 95%, and heat to a temperature of 80°C, at which time the cyclohexane reflux starts to react. After reacting for 1h, add reaction accelerator methanol solution 60ml in reactor, reaction system temperature reduces gradually, and material viscous state alleviates, and then every two hours adds methanol solution identical with the first addition in still, keeps like this Reflux state reaction 5.5h, the condensation reaction is over. Then add NaHCO to the reactor 3 3.5g, after the pH of the reaction system was made to be 9, the temperature was raised and the cyclohexane was evaporated for recycling. The crude DMDBS obtained was washed, filtered, dried and pulverized...

Embodiment 3

[0024] In a 1L reaction kettle equipped with a condenser and an oil-water separator paddle stirrer, add 18 g of sorbitol with a content of 98%, 1.5 g of p-toluenesulfonic acid, trimethylhexadecyl chloride Ammonium 3.0g, toluene 325ml, then start the agitator, and add 29g of 3,4-dimethylbenzaldehyde with a content of 95%, and heat to a temperature of 110°C. At this time, the toluene reflux starts to react. After 1 hour of reaction, once Add 180ml of reaction accelerator methanol solution in the reactor, the temperature of the reaction system decreases gradually, and the viscous state of the material is relieved, then every two hours, add the same methanol solution with the first addition in the kettle, so that the reflux state is maintained for 5.5 h, the condensation reaction is over. Then add NaHCO to the reactor 3 3.5g, after the pH of the reaction system was 8, the toluene was evaporated by heating up for recycling, and the crude DMDBS obtained was washed, filtered, dried, ...

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

PropertyMeasurementUnit
melting pointaaaaaaaaaa
purityaaaaaaaaaa
purityaaaaaaaaaa
Login to view more

Abstract

The present invention relates to a method for synthesizing 1,3:2,4-di(3,4-dimethyl) benzylidene sorbitol. Said method includes the following steps: successively adding sorbitol, catalyst, emulsifyingagent and solvent into a reactor, stirring them and at the same time adding 2,4-dimethylbenzaldehyde, heating to 70-115deg.C, making condensation separation, solvent refluxing reaction for 1 hr, stirring speed is 100-130 rpm, slowly-adding accelerating agent, making further reaction for 5-6hr, regulating system and making it into alkalescence, recovering solvent, making the obtained crude produceundergo the processes of washing, faltering and drying so as to obtain the invented product.

Description

technical field [0001] The invention relates to a method for synthesizing high-purity 1,3:2,4-di(3,4-dimethyl)benzylidene sorbitol. Background technique [0002] It is well known that dibenzylidene sorbitol (DBS, hereinafter the same) and its derivative nucleating agents have a good improvement effect on polyolefin resins. After adding such substances, the haze of the prepared polypropylene (PP) sheet is significantly reduced, and the transparency, heat distortion temperature and rigidity of the product are all significantly improved, which can improve its commercial value and market competitiveness. [0003] Japanese Patent JP81 / 00105, European Patent EP0139917A, Chinese Patent CN1087354AT and CN1351013A all report high selectivity and high yield to prepare dibenzylidene sorbitol (first generation product), and di-p-methylbenzyl sorbitol ( MDBS, the second generation product) synthetic method of polycondensate. It is based on sorbitol and benzaldehyde, p-toluene or p-chlo...

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 Patents(China)
IPC IPC(8): C07D493/04C07D319/00
Inventor 张跃刘宇严生虎王勋章王芳郑志强
Owner BC P INC CHINA NAT PETROLEUM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap