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Method for preparing oleic acid esters by using solid super acid as catalyst

A solid super acid and catalyst technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of ineffective replacement of sulfuric acid, low yield, etc., to reduce energy consumption and reaction selection. Good performance, reducing emissions

Inactive Publication Date: 2008-07-30
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a kind of method that utilizes solid superacid as catalyst to prepare oleic acid alcohol ester, to overcome the low yield that prior art exists, can not effectively reach the problem that replaces sulfuric acid as catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: SO 4 2- / ZrO 2 Preparation of solid superacid catalyst (SZ). ZrOCl 2 ·8H 2 O as raw material to prepare SO 4 2- / ZrO 2 Solid superacid, weighed ZrOCl 2 ·8H 2 O was dissolved in deionized water to prepare three kinds of solutions with mass percentage of 6%, 50% and supersaturation, then moved into the fume hood, and added 28% ammonia solution dropwise while stirring on the magnetic stirrer until white flocculent precipitate appeared , adjust the pH of the solution to 9-10, and then adjust different temperatures in a blast drying oven to dry for 12-24 hours. Subsequently, this ZrO 2 The carrier was added to a 0.5mol / L sulfuric acid accelerator, ultrasonically impregnated for 30min, and calcined at 550°C for 3h, and the prepared samples were placed in a desiccator for later use.

Embodiment 2

[0018] Example 2: SO 4 2- / ZrO 2 -TiO 2 Preparation of solid superacid catalyst (SZT). Aspirate TiCl with a needle in a fume hood 4 Quickly pour into a beaker filled with distilled water to make 17% (w / v) TiCl 4 Solution, mixed with the supersaturated zirconium oxychloride solution in the ratio of n(Ti):n(Zr)=4.0:1.0, slowly added 28% ammonia water dropwise under stirring until a large amount of white flocculent precipitates were formed, adjusted When the pH of the solution reaches 9, continue to stir for 2 hours at room temperature, age for 24 hours at -15°C, and filter under reduced pressure. mol / L AgNO 3 Chloride ions (Cl - ) until it exists. Dry the filter cake at 105°C for 24 hours, grind it into powder below 100 mesh, add it to 0.5mol / L sulfuric acid accelerator, impregnate it in ultrasonic for 20 minutes, and filter it with suction. Dry the filter cake at 100°C, then place it in a muffle furnace, slowly raise the temperature to 550°C, roast for 3 hours, take it...

Embodiment 3

[0019] Example 3: SO 4 2- / ZrO 2 -La 3+ Preparation of solid superacid catalyst (SZL). Take a supersaturated solution of zirconium oxychloride, and slowly add 28% ammonia water dropwise under stirring until a large amount of white flocculent precipitates are formed. Adjust the pH of the solution to 9, then add 0.08% to 0.1% lanthanum nitrate, and continue to stir at room temperature for 2 hours to allow it to fully react. The intermediate product was aged at -15°C for 24 hours, filtered under reduced pressure, and the filter cake was redissolved in deionized water, stirred for 30 minutes until the precipitate was mixed evenly, and continued to be filtered by suction, and the operation was repeated until 0.01mol / L AgNO 3 Chloride ions (Cl - ) until it exists. Dry the filter cake at 105°C for 24 hours, grind it into a powder below 100 mesh, add it to a 0.5mol / L sulfuric acid accelerator, impregnate it with ultrasonic waves for 40 minutes, and filter it with suction. Dry t...

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PUM

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Abstract

The invention relates to a method for manufacturing oleic acid ester by using solid superacid as catalyst. The invention can overcome problems existing in the prior art that products are impure, yield coefficient is low and the prior art can not achieve the object of replacing sulphuric acid as catalyst. For overcoming the problems existing in the prior art, the technical proposal provided by the invention is that: the method for manufacturing oleic acid ester by using solid superacid as catalyst is characterized in that ZrO2 carrier is added into sulphuric acid accelerator to carry out ultrasonic wave dipping in all the process for preparing the solid superacid; after dipping for 20 to 40 minutes, the obtained substance is filtered and parched; as the catalyst, the dosage of the solid superacid is 0.05 percent to 0.5 percent of the quality of the oleic acid. Comparing with the prior art, the invention has the advantages that: the preparation cycle of the solid superacid is shortened and the activity is enhanced; side effect does not easily occur by using the solid superacid as the catalyst; the production technique is simplified. And the invention has convenient post treatment and low energy consumption, and is safe as well as reliable, which suits for the sustainable development requirement of chemical industry.

Description

Technical field: [0001] The invention relates to a method for preparing oleic acid alcohol ester by using solid superacid as a catalyst. Background technique: [0002] In recent years, because people's awareness of environmental protection has increased, and oil products have the advantages of low toxicity, low irritation and easy biodegradation, more and more attention has been paid to the synthesis of surfactants from oleic acid. Polyethylene glycol oleate and high-carbon alcohol oleate in alcohol oleate are two important industrial reaction intermediates. If they are further derivatized, they can be used to synthesize various surfactants, lubricating oils, oil additives, etc. , so it has a wide range of industrial application value. At present, the method for industrially producing alcohol esters of oleic acid is mainly the direct esterification of fatty acids and alcohols. In the traditional production process, inorganic acids represented by concentrated sulfuric acid ...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/58B01J27/053
Inventor 罗晓民张晓镭强涛涛任龙芳
Owner SHAANXI UNIV OF SCI & TECH
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