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Solid acid catalyst for catalyzing esterification reaction of pentaerythritol and stearic acid and preparation method of solid acid catalyst

A technology of solid acid catalyst and stearate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the problem of high yield of pentaerythritol stearate and high yield of pentaerythritol stearate. Low cost, complex catalyst preparation methods, etc., to achieve the effects of uniform grain size, rich acid content, and short preparation time

Active Publication Date: 2021-06-18
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Purpose of the invention: the present invention provides a catalyst for the synthesis of pentaerythritol stearate aimed at problems such as complex catalyst preparation methods, difficult catalyst separation, and low yield of pentaerythritol stearate in the current preparation process of pentaerythritol stearate The preparation method of the catalyst, the preparation method of the catalyst is simple, easy to separate from the product, and the pentaerythritol stearate productive rate is high

Method used

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  • Solid acid catalyst for catalyzing esterification reaction of pentaerythritol and stearic acid and preparation method of solid acid catalyst
  • Solid acid catalyst for catalyzing esterification reaction of pentaerythritol and stearic acid and preparation method of solid acid catalyst
  • Solid acid catalyst for catalyzing esterification reaction of pentaerythritol and stearic acid and preparation method of solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] With 4.29g zirconium nitrate (consumption is represented by ZrO 2 Calculation), 9.14g tetrapropyl ammonium hydroxide (TPAOH), 2.55g ammonia water (the amount is expressed as NH 3 Calculation), 9g deionized water, ZrO in molar ratio 2 :TPAOH:NH 3 :H 2 O=1:4.5:15:50 mixed, at room temperature with a stirring rate of 50r / min stirring for 1h, to obtain solution a; according to ZrO 2 :SnO 2 =1:2 molar ratio, with 5.34g sodium stannate (consumption is based on SnO 2 Calculation) and 10.8g deionized water, in molar ratio for SnO 2 :H 2 O=1:30 mixing, stirring at room temperature at a stirring rate of 50r / min for 1h to obtain solution b; adding solution b dropwise to solution a at a rate of 0.6mL / min, and stirring at a rate of 65°C Stir at 50r / min for 1h to form a sol-gel; transfer the sol-gel to a supercritical reactor, feed carbon dioxide gas into the reactor, and make the reactor reach a supercritical environment of 35°C and a pressure of 8MPa, and Keep for 5 hours, ...

Embodiment 2

[0028] With 4.29g zirconium nitrate (consumption is represented by ZrO 2 Calculation), 14.7g tetraethylammonium hydroxide (TEAOH), 3.4g ammonia water (the amount is expressed as NH 3 Calculation), 27g deionized water, ZrO in molar ratio 2 :TEAOH:NH 3 :H 2 O=1:10:20:150 mixing, stirring at room temperature at a stirring rate of 60r / min for 3h to obtain solution a; according to ZrO 2 :SnO 2 =1:5 mol ratio, with 9.5g stannous chloride (consumption is based on SnO 2 Calculation) and 40.5g deionized water, in molar ratio for SnO 2 :H 2 O=1:45 mixing, stirring at room temperature at a stirring rate of 60r / min for 3h to obtain solution b; adding solution b dropwise to solution a at a rate of 0.8mL / min, and stirring at a rate of 80°C Stir at 60r / min for 3h to form a sol-gel; transfer the sol-gel to a supercritical reactor, feed carbon dioxide gas into the reactor, and make the reactor reach a supercritical environment of 100°C and a pressure of 15MPa, and Keep it for 1h, filte...

Embodiment 3

[0030] With 3.27g zirconium acetate (consumption is represented by ZrO 2Calculation), 13.0g tetrabutylammonium hydroxide (TBAOH), 3.06g ammonia water (the amount is expressed as NH 3 Calculation), 18g deionized water, ZrO in molar ratio 2 :TEAOH:NH 3 :H 2 O=1:5:18:100 mixing, at room temperature, stirring at a stirring rate of 60r / min for 3h to obtain solution a; according to ZrO 2 :SnO 2 =1:3 mol ratio, with 5.7g stannous chloride (consumption is based on SnO 2 Calculation) and 27g deionized water, in molar ratio for SnO 2 :H 2 O=1:50 mixing, stirring at room temperature at a stirring rate of 70r / min for 2h to obtain solution b; adding solution b dropwise to solution a at a rate of 1.0mL / min, and stirring at a rate of 85°C Stir at 70r / min for 2h to form a sol-gel; transfer the sol-gel to a supercritical reactor, feed carbon dioxide gas into the reactor, and make the reactor reach a supercritical environment of 130°C and a pressure of 20MPa, and Keep for 5 hours, filte...

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Abstract

The invention discloses a solid acid catalyst for catalyzing esterification reaction of pentaerythritol and stearic acid and a preparation method of the solid acid catalyst. The preparation method comprises the following steps of mixing a zirconium source, a structure-directing agent, ammonia water and deionized water, and uniformly stirring at room temperature to obtain a solution a, meanwhile, mixing a tin source with deionized water, and uniformly stirring at room temperature to obtain a solution b, dropwise adding the solution b into the solution a, and stirring at a certain temperature to form sol-gel, transferring the obtained sol-gel into a supercritical reaction kettle for crystallization reaction, and filtering the obtained crystallization product, washing, drying, and roasting at 500 DEG C for 1-3 hours to obtain the product. The solid acid catalyst disclosed by the invention is large in specific surface area and is in full contact with an acidic active site, so that the catalyst has relatively high catalytic activity, the temperature required by reaction is relatively low, and the reaction energy consumption is reduced; the acid strength is high, the esterification reaction of pentaerythritol and stearic acid is facilitated, and the raw material conversion rate and the yield of the target product pentaerythritol stearate are high; and the acid value of the product is small.

Description

technical field [0001] The invention belongs to the technical field of preparation of solid acid catalytic materials, in particular to a catalyst for catalyzing the esterification reaction of pentaerythritol and stearate and a preparation method thereof. Background technique [0002] Pentaerythritol stearate is a white hard high melting point wax, soluble in ethanol, benzene and chloroform, insoluble in water. It can be widely used as an auxiliary heat stabilizer, plasticizer, lubricating brightener in the rubber and plastic industries, and can also be used as a transparent lubricant for calendered film and blown film. It is especially suitable for applications that require thermal stability and excellent mold release. working conditions. [0003] The traditional preparation method of pentaerythritol stearate is to use pentaerythritol and stearic acid as raw materials under the action of an acidic or basic catalyst, and generate by esterification under high temperature cond...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/14B01J35/10B01J35/02C07C67/08C07C69/33B01J35/00
CPCB01J23/14C07C67/08B01J35/617B01J35/40B01J35/615C07C69/33Y02P20/54
Inventor 丁建飞丁薇张义东邵荣许伟
Owner YANCHENG INST OF TECH