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Preparation method of heat conduction oil

A technology of heat-conducting oil and benzyl chloride, which is applied in the field of heat-conducting oil preparation, can solve the problems of frequent regeneration, non-reuse, strong corrosion of concentrated sulfuric acid, etc., and achieve the effect of improving yield

Inactive Publication Date: 2015-07-15
中化化工科学技术研究总院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Studies have shown that although concentrated sulfuric acid or solid acid catalysts are used as catalysts, they have higher catalytic activity, but they also have the following limitations: when concentrated sulfuric acid is used as catalysts, there is a large amount of concentrated sulfuric acid and cannot be recycled, resulting in a large amount of (Producing 1 ton of insulating oil will produce about 0.5 tons of waste acid and 1 ton of acid-containing wastewater), concentrated sulfuric acid is highly corrosive, difficult to handle, and cannot be reused; when using solid acid as a catalyst, there will be solid acid The catalyst preparation process is complex, expensive and requires frequent regeneration during the production process, which makes the production cost of heat transfer oil high, thus limiting its popularization and use

Method used

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  • Preparation method of heat conduction oil
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preparation example Construction

[0011] The preparation method of the heat conduction oil provided by the invention comprises that the general formula is Bu 3 P + R 2 R 1 - / nZnCl 2 / mLaCl 3 In the presence of the quaternary phosphonium salt ionic liquid composite catalyst, under stirring conditions, toluene is contacted with benzyl chloride, and the contact conditions include a temperature of 90-110 ° C and a time of 5-8 hours, wherein R 1 is halogen, R 2 for C 10 -C 18 straight-chain or branched-chain alkyl, n is 1-5, and m is 0.01-0.5. Preferably, R 1 is chlorine atom or bromine atom, R 2 for C 12 -C 16 straight-chain alkyl, n is 2-4, m is 0.01-0.1, and n and m represent moles.

[0012] Among them, n represents relative to 1 mole of Bu 3 P + R 2 R 1 - , ZnCl 2 The number of moles is 1-5; m means relative to 1 mole of Bu 3 P + R 2 R 1 - , LaCl 3 The number of moles is 0.01-0.5. The halogen can be a chlorine atom, a bromine atom, a fluorine atom or an iodine atom; the C 10 -C 18 S...

preparation example 1

[0031] This preparation example is used to illustrate the quaternary phosphonium salt ionic liquid composite catalyst provided by the present invention and its preparation method.

[0032] 1mol of dodecyltributylphosphonium chloride (purchased from Beijing Ruishibang Fine Chemical Technology Co., Ltd., with a water content of 50% by weight) was stirred and mixed with 500mL of toluene, and heated to 90°C for vacuum distillation until Until there is no effluent at this temperature;

[0033] Put 2mol of zinc chloride and 0.06mol of lanthanum chloride into the oven respectively, and dry at 110°C for 30min;

[0034] Under the protection of nitrogen and under stirring conditions, mix the dodecyltributylphosphonium chloride, zinc chloride and lanthanum chloride treated by the above method evenly, and raise the temperature to 140°C and react for 2 hours , to obtain the quaternary phosphonium salt ionic liquid composite catalyst C1.

preparation example 2

[0036] This preparation example is used to illustrate the quaternary phosphonium salt ionic liquid composite catalyst provided by the present invention and its preparation method.

[0037] Stir and mix 1 mol of tetradecyltributylphosphonium chloride (purchased from Beijing Ruishibang Fine Chemical Technology Co., Ltd., with a water content of 50% by weight) and 500mL of toluene, and heat to 90°C for vacuum distillation until Until there is no effluent at this temperature;

[0038] Put 3mol zinc chloride and 0.02mol lanthanum chloride into the oven respectively, and dry at 110°C for 30min;

[0039] Under the protection of nitrogen and under stirring conditions, mix the tetradecyltributylphosphonium chloride, zinc chloride and lanthanum chloride treated by the above method evenly, and raise the temperature to 120°C and react for 4 hours , to obtain the quaternary phosphonium salt ionic liquid composite catalyst C2.

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Abstract

The invention provides a preparation method of heat conduction oil, and the preparation method comprises the following steps: in the presence of a quaternary phosphonium salt ionic liquid composite catalyst with a general formula of Bu3P<+>R2R1<-> / nZnCl2 / mLaCl3, enabling toluene to contact with benzyl chloride while stirring, wherein the contact conditions are as follows: the temperature is 90-110 DEG C and the time is 5-8 hours; R1 is halogen, R2 is C10-C18 straight-chain or branched-chain alkyl group, n is 1-5, and m is 0.01-0.5. By adopting the method provided by the invention to prepare heat conduction oil, the yield of the reaction product as well as the yield of monobenzyl toluene and bisbenzyl toluene in the reaction product can be improved. Moreover, after the reaction, the quaternary phosphonium salt ionic liquid composite catalyst can be effectively recycled to realize cyclic utilization while the environmental pollution is avoided, and the production cost is reduced.

Description

technical field [0001] The invention relates to a preparation method of heat conduction oil. Background technique [0002] Ionic liquids are a class of environmentally friendly solvents that are generally considered to have broad application prospects and can replace traditional organic solvents. At present, the application fields of ionic liquids mainly include: polymerization reaction, selective alkylation, amination reaction, acylation reaction, esterification reaction, rearrangement reaction of chemical bonds, catalytic hydrogenation reaction at room temperature and normal pressure, cyclic reaction of olefins Oxidation reactions, etc., and show the advantages of fast reaction speed, high conversion rate and selectivity, and the catalytic system can be recycled and reused. The ionic liquid itself has the characteristics of low vapor pressure and stable chemical properties. During the chemical reaction process, no harmful gas that pollutes the atmosphere will be produced,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/86C07C15/16C09K5/10
CPCY02P20/584
Inventor 伍振毅殷冬媛赵新王果果梁睿赵瑞英
Owner 中化化工科学技术研究总院有限公司