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A kind of pre-esterification method for preparing biodiesel

A technology of biodiesel and pre-esterification, applied in chemical instruments and methods, biofuels, fatty acid esterification, etc., can solve the problems of unsuitability for industrial production, low conversion rate, complicated process, etc., to increase the probability of exposure and Mass transfer efficiency, increase reaction efficiency and conversion rate, and reduce the effect of acid value of raw materials

Active Publication Date: 2021-08-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The literature "Study on Pre-esterification of Waste Oil Catalyzed by Solid Composite Acid" and "Research on Preparation of Biodiesel from Oil with High Acid Value" reported the research on the pre-esterification of oil in the tank method. The process is complicated and the conversion rate is low. And it cannot be carried out continuously with the subsequent transesterification reaction, which is not conducive to industrial application
The literature "Research on the Pre-esterification of Tung Oil Catalyzed by Solid Acid" uses ion exchange resin as the catalyst, and the fixed bed continuous reaction method, the acid value is reduced to 0.8KOHmg / g, which has the advantages of fast reaction and continuous performance, but in the process of reaction The water produced in can convert the H in the sulfonic acid group in the catalyst + Carried away, leading to catalyst deactivation and shortening service life
[0005] Chinese patent CN101020863 discloses a pre-esterification process using methanol vapor and grease reaction. Although the acid value can be reduced to 0.5 KOHmg / g, the reaction is still carried out in the reactor, and the amount of methanol vapor is large, and the recovery energy consumption is relatively high. High, not suitable for industrial production; Chinese patent CN103031216A discloses a pre-esterification process for producing biodiesel from waste oil, using concentrated sulfuric acid as a catalyst, which is likely to cause equipment corrosion and environmental pollution

Method used

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  • A kind of pre-esterification method for preparing biodiesel
  • A kind of pre-esterification method for preparing biodiesel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of modified ion exchange resin catalyst: a: Wash 150 grams of styrene-based strongly acidic cation exchange resin with deionized water for 5 times, each time for 10 minutes, and dry it in a vacuum oven at 90°C for 4 hours; b : Put the dried strongly acidic cation exchange resin into a 2mm thick steel mesh bag, spread it flat in an ultrasonic vibrator with a vibration frequency of 58kHz, and use an atomizing nozzle with a 35% mass percentage of phosphotungstic acid aqueous solution and nitrogen Spray impregnation for 2 hours, spray distance 1cm, spray pressure 0.05MPa; c: After washing, dry in a vacuum oven at 90°C for 6 hours, and bake the dried ion exchange resin at 210°C for 8 hours; d: Then Treat the resin with 20% aqueous solution of phosphotungstic acid according to the method of b. After washing, dry it in a vacuum oven at 80°C for 6 hours, and roast the dried ion exchange resin at 200°C for 8 hours to obtain the loaded type heteropolyacid catalyst...

Embodiment 2

[0036] (1) Preparation of modified ion exchange resin catalyst: a: Wash 150 grams of styrene-based strongly acidic cation exchange resin with deionized water for 5 times, each time for 10 minutes, and dry it in a vacuum oven at 90°C for 6 hours; b : Put the dried strong acidic cation exchange resin into a 3mm thick steel mesh bag, lay it flat in an ultrasonic vibrator, the vibration frequency is 59kHz, and use an atomizing nozzle to spray phosphotungstic acid aqueous solution with a mass percentage of 35% and nitrogen Spray impregnation for 2 hours, spray distance 2cm, spray pressure 0.07MPa; c: After washing, dry in a vacuum oven at 90°C for 6 hours, and bake the dried ion exchange resin at 220°C for 8 hours; d: Then Treat the resin with 15% phosphotungstic acid aqueous solution according to the method b, after washing, dry it in a vacuum oven at 80°C for 6 hours, and roast the dried ion exchange resin at 200°C for 8 hours to obtain the supported type heteropolyacid catalyst....

Embodiment 3

[0039] (1) Preparation of modified ion exchange resin catalyst: a: Wash 150 grams of styrene-based strongly acidic cation exchange resin with deionized water for 5 times, each time for 10 minutes, and dry it in a vacuum oven at 90°C for 6 hours; b : Put the dried strongly acidic cation exchange resin into a 3mm thick steel mesh bag, lay it flat in an ultrasonic vibrator with a vibration frequency of 60kHz, and use an atomizing nozzle with a 45% mass percentage of phosphotungstic acid aqueous solution and nitrogen Spray impregnation for 2 hours, spray distance 2cm, spray pressure 0.06MPa; c: After washing, dry in a vacuum oven at 90°C for 6 hours, and bake the dried ion exchange resin at 220°C for 8 hours; d: Then Treat the resin with 20% aqueous solution of phosphotungstic acid according to the method of b. After washing, dry it in a vacuum oven at 80°C for 6 hours, and roast the dried ion exchange resin at 200°C for 8 hours to obtain the loaded type heteropolyacid catalyst. ...

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Abstract

A method for preparing biodiesel pre-esterification, using a fixed bed tubular reactor, the middle part of the reactor is a catalyst bed, the upper part is provided with a partition along the axial direction, the lower end of the partition extends into the catalyst bed, and does not completely penetrate the catalyst bed layer, separator and catalyst bed divide the reactor into three parts, the upper feed section and the discharge section are on both sides of the separator, and the lower feed section is below the catalyst bed; tung oil and methanol are fed from the top as feed I The raw material inlet of the feed section enters, methanol and nitrogen enter from the raw material inlet of the lower feed section as feed II, and the feed I undergoes a pre-esterification reaction on the catalyst bed, and the reacted material is combined with the bottom-up feed II Mixing, further reaction, the product is discharged from the discharge port of the discharge section. The reaction mode of the above method makes the material react more fully, improves the conversion rate of the pre-esterification reaction, greatly reduces the acid value of the raw material, and feeds the upper end to reciprocate through the catalyst bed, so that the reaction is more sufficient and the conversion rate of the fatty acid is improved.

Description

technical field [0001] The invention relates to a pre-esterification method for preparing biodiesel, in particular to a pre-esterification method using tung oil with high acid value and methanol as raw materials. Background technique [0002] In the mid-to-late 1980s, as the two major problems of environmental protection and oil resource depletion attracted more and more attention, biodiesel once again became the most popular research topic to solve the energy crisis and environmental pollution. Western developed countries such as the United States, France, and Italy successively A special biodiesel research institution has been established, and a lot of manpower and material resources have been invested in the research of biodiesel. Biodiesel is a non-toxic, biodegradable, renewable clean fuel that can replace ordinary petroleum diesel. It can be mixed with diesel in any proportion or used directly on diesel engines, and can reduce greenhouse gas emissions and reduce air po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J8/02B01J31/34B01J31/18C10L1/02C11C3/10
CPCB01J8/02B01J27/188B01J31/08B01J31/34C10L1/02C11C3/10Y02E50/10
Inventor 刘野霍稳周吕清林李花伊
Owner CHINA PETROLEUM & CHEM CORP
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