Method for preparing tributyl citrate by using tubular reactor

A technology of tributyl citrate and tubular reactor, applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation and other directions, can solve the difficulty of refining and recycling reaction products, long production cycle, complicated process, etc. problems, to achieve the effect of product quality and stability, significant economic benefits, and obvious environmental benefits

Active Publication Date: 2017-05-17
NANJING POLYTECHNIC INSITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its production method is that citric acid and n-butanol react to generate tributyl citrate in the presence of a catalyst and a water-carrying agent. The commonly used catalyst is an inorganic or organic acid (the most commonly used is concentrated sulfuric acid), and the water-carrying agent is positive Butanol itself is produced through dealcoholization, neutralization, water washing, stripping, decolorization, pressure filtration, rectification and other processes; although sulfuric acid is cheap and has high catalytic activity, it has many disadvantages: long production cycle and low conversion rate; And because of the dehydration, esterification and oxidation of sulfuric acid, there are many by-products, which all bring difficulties to the refining and recovery of the reaction product; After alkali neutralization, water washing, and removal of sulfuric acid as a catalyst, the process is complicated, three wastes are generated, and the product is lost; in addition, sulfuric acid also seriously corrodes equipment and increases production costs; produce three wastes pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put the mixture of butanol and citric acid (the molar ratio is 3.0) (in the storage tank at 80°C and mix evenly) continuously into the Φ6×10000 10% copper p-toluenesulfonate / A.C. solid catalyst (10-20 mesh) Carry out reaction in the tubular reactor, reaction temperature 100 ℃, material residence time is 1.5h, reaction pressure 1.0MPa; Pump into butanol (its molar ratio is 1.5) in the back third place of tubular reactor, reaction When the mixture leaves the tubular reactor, the citric acid conversion rate is 99.3%; the reacted mixture enters the neutralization reactor, and is neutralized by adding saturated lime water to remove unreacted trace citric acid, and the pH in the reactor tank is controlled. is 8.0. The generated solid by-products are removed through a tubular filter; two tubular filters are connected in parallel, and when one tubular filter is full of solids, switch to another tubular filter; or use other equipment for continuous filtration ; The mixed soluti...

Embodiment 2

[0018] Put the mixture of butanol and citric acid (the molar ratio is 4.0) (in the storage tank at 80°C and mix well) continuously into the Φ6×10000 tube filled with 20% p-toluenesulfonic acid / A.C. solid catalyst (10-20 mesh) The reaction is carried out in a tubular reactor, the reaction temperature is 80°C, the material residence time is 2.0h, and the reaction pressure is 3.0MPa; butanol (its molar ratio is 1.0) is pumped into the last third of the tubular reactor, and the reaction When the mixture leaves the tubular reactor, the citric acid conversion rate is 99.0%; the reacted mixture enters the neutralization reactor, and is neutralized by adding saturated lime water to remove unreacted trace citric acid, and the pH in the reactor tank is controlled. is 7.5. The generated solid by-products are removed through a tubular filter; two tubular filters are connected in parallel, and when one tubular filter is full of solids, switch to another tubular filter; or use other equipme...

Embodiment 3

[0020] Put the mixture of butanol and citric acid (the molar ratio is 3.5) (in the storage tank at 80°C and mix well) continuously into the Φ6×10000 tubular reactor equipped with niobium pentoxide solid catalyst (10-20 mesh) Carry out the reaction, the reaction temperature is 170°C, the material residence time is 0.5h, and the reaction pressure is 1.0MPa; butanol (its molar ratio is 1.0) is pumped into the last third of the tubular reactor, and the reaction mixture leaves the tubular reactor The conversion rate of citric acid in the reactor is 99.6%; the reacted mixture enters the neutralization reactor, and is neutralized by adding saturated lime water to remove unreacted trace citric acid, and the pH in the reactor is controlled to be 9.0. The generated solid by-products are removed through a tubular filter; two tubular filters are connected in parallel, and when one tubular filter is full of solids, switch to another tubular filter; or use other equipment for continuous filt...

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PUM

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Abstract

The invention discloses a method for green and continuous production of tributyl citrate. A tubular reactor (containing an efficient soil catalyst) is used to realize efficient conversion of citric acid and butanol and combined with a continuous impurity removal technology and a continuous rectification technology, continuous production of the product is realized, the purity of the product, namely, tributyl citrate, is higher than or equal to 99.0, and the yield of the main product, namely, tributyl citrate, is higher than 98.0%, and no pollution is caused in the whole process.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing tributyl citrate using a tubular reactor. Background technique [0002] DOP (dioctyl phthalate) (DBP) has good compatibility with most synthetic resins and rubbers used in industry, and also has good comprehensive performance, good mixing performance, high plasticizing efficiency, and low volatility. Low temperature, good softness at low temperature, water resistance, high electrical performance, good heat resistance and weather resistance, etc., so it is the most widely used general-purpose plasticizer, mainly used in the processing of polyvinyl chloride resin, It can also be used in the processing of high polymers such as chemical resin, acetic acid resin, ABS resin and rubber, and can also be used in the manufacture of paint, dyes, dispersants, etc. DOP plasticized PVC can be used to manufacture artificial leather, agricultural fil...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/60C07C67/54C07C69/704C07C51/41C07C59/265
CPCC07C51/412C07C67/08C07C67/54C07C67/60C07C69/704C07C59/265
Inventor 吴永忠张晶
Owner NANJING POLYTECHNIC INSITUTE
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