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Preparation method of vinyl distearamide

A technology of vinyl bisstearamide and stearic acid, which is applied in the chemical industry, can solve the problems of lowering the reaction temperature, easy yellowing of the color, complicated process, etc., and achieves the effect of reducing side reactions, reducing chroma, and simple process

Active Publication Date: 2016-07-20
GUANGZHOU CARDLO BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The synthesis method of EBS mainly contains four kinds: 1) fatty acid ester and amine compound react to generate EBS, the product purity of this method gained is higher, but energy consumption is big, the treatment of alcohol in the esterification reaction of fatty acid and reaction process makes process Complicated, long procedure; 2) acid chloride and amine compound react to prepare EBS, reduce reaction temperature, product purity is high, color and luster is good, but production cost is high, technological process is long; 3) the hydrolysis of nitrile cyanide compound, because cyanide is poisonous, The production process pollutes the environment seriously, and this method has been eliminated; 4) EBS is prepared by the reaction of fatty acids and amine compounds. This method has simple process, mild reaction conditions, easy-to-get raw materials, and less waste. It is currently the main EBS synthesis route in China.
Chinese patent application CN102964266A discloses a high-yield synthesis process for ethylene bisstearamide, using stearic acid and ethylenediamine as reaction materials, phosphoric acid and acetic anhydride as catalysts, and sulfite as an antioxidant. The invention synthesizes The process is simple, the operation is convenient, and the three wastes are less, but the color is darker and the melting range of the product is wider
[0004] The method for preparing EBS by the reaction of stearic acid and ethylenediamine is simple and easy to produce on a large scale, but the prepared EBS product often has problems such as low product purity, easy yellowish color, high chroma, and wide melting range. The synthesis process needs to be improved

Method used

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  • Preparation method of vinyl distearamide

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1 prepares p-toluenesulfonic acid / SAPO-34 supported solid acid catalyst

[0020] Dissolve p-toluenesulfonic acid in deionized water, prepare a p-toluenesulfonic acid solution with a mass fraction of 30% as an impregnation solution, use SAPO-34 molecular sieve after roasting at 500°C for 3.5h as a carrier, and adjust the liquid-solid ratio 2.0mL / g is placed in p-toluenesulfonic acid solution, impregnated by ultrasonic impregnation, and the impregnation time is 12h; the above impregnated material is dried at 120°C for 12h, and roasted in an air atmosphere at 550°C in a muffle furnace for 4h , to obtain p-toluenesulfonic acid / SAPO-34 supported solid acid catalyst.

Embodiment 2

[0021] Embodiment 2 prepares phosphoric acid / SiO2-Al2O3 supported solid acid catalyst

[0022] S1: Take aluminum nitrate and dissolve it in absolute ethanol at a solid-to-liquid ratio of 0.10 g / mL to prepare an ethanol solution of aluminum nitrate, add 40% of its volume to tetraethyl orthosilicate and 15% of its volume to 30% of its volume fraction Aqueous urea solution, stirred for 10 minutes, stirred and refluxed at 80°C to form a gel, dried at 120°C for 8 hours, and calcined in a muffle furnace at 550°C for 3 hours to obtain SiO 2 -Al 2 o 3 composite oxides;

[0023] S2: SiO prepared from S1 with 55% phosphoric acid solution as the impregnating solution 2 -Al 2 o 3 The composite oxide is used as a carrier and placed in a phosphoric acid solution at a liquid-solid ratio of 1.0mL / g, and is impregnated by ultrasonic impregnation for 16 hours; the impregnated material is dried at 120°C for 12 hours, and placed in a muffle furnace in an air atmosphere Calcined at 550°C for...

Embodiment 3

[0024] Embodiment 3 prepares vinyl bis stearamide

[0025] Add stearic acid and a composite antioxidant of 0.28% stearic acid mass into the reactor, and feed N while stirring. 2 After 10 minutes, slowly raise the temperature to 100°C to melt all the stearic acid, add ethylenediamine and a composite catalyst of 0.20% by mass of stearic acid, react at a constant temperature for 2 hours, then slowly raise the temperature to 180°C, and react at a constant temperature for 4 hours to make it The dehydration reaction is carried out, and the water generated during the reaction is composed of N 2 Take out, stop the reaction, cool to 160°C and discharge. Among them, the molar ratio of stearic acid and ethylenediamine is 1:0.58; the mass ratio of antioxidant 1076, antioxidant DLTDP and antioxidant T501 in the composite antioxidant is 0.20:0.36:1; The p-toluenesulfonic acid / SAPO-34 supported solid acid catalyst and phosphoric acid / SiO that example 1 and embodiment 2 make 2 -Al 2 o 3 ...

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Abstract

The invention belongs to the technical field of chemical engineering and particularly relates to a preparation method of vinyl distearamide. The preparation method uses stearic acid and ethylenediamine as reacting raw materials, uses a composite antioxidant prepared by compounding an antioxidant 1076, an antioxidant DLTDP and an antioxidant T501 as a reacting antioxidant and uses a composite catalyst prepared by compounding a p-Toluene sulfonic acid / SAPO-34 supported solid acid catalyst and a phosphoric acid / SiO2-Al2O3 supported solid acid catalyst as a reaction catalyst. The preparation method of the vinyl distearamide is simple in process, no 'three wastes' emission is produced in the process of preparing the vinyl distearamide, the yield is high, and the prepared vinyl distearamide is high in purity, low in chromaticity and narrow in melting range.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of vinylbisstearamide. Background technique [0002] Fatty acid bisamide compounds are widely used in various polymer materials and wood-plastic materials, and have multiple functions such as lubrication, mold release, anti-adhesion, antistatic, promotion of pigment dispersion, and increase of product surface gloss. Vinyl bisstearamide, also known as N,N'-ethylene bisstearamide (EBS), is one of the earliest fatty bisamide products developed. The EBS structure contains polar amide groups and two long carbon chains The hydrophobic group makes it have the characteristics of high-temperature lubricity and low-temperature anti-sticking properties, plus its combination with synthetic resins such as acrylonitrile-butadiene-styrene polymer (ABS), polyvinyl chloride, phenolic resin, polystyrene Ethylene has good compatibility and is a multi-func...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C233/36
CPCC07C231/02C07C233/36
Inventor 徐怀义马银官徐伟伟
Owner GUANGZHOU CARDLO BIOCHEM TECH
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