Technological method for preparing 1, 3-propylene glycol by adopting glycerin and hydrogen

A process method and technology for propylene glycol, which are applied in the field of hydrogenation to prepare 1,3-propylene glycol, can solve the problems of high energy consumption, poor reaction stability and high reaction temperature, and achieve the effects of stable catalyst, mild reaction conditions and increased production rate.

Inactive Publication Date: 2014-01-22
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above methods for preparing 1,3-propanediol by catalytic hydrogenation of glycerin, or the reaction temperature is relatively

Method used

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  • Technological method for preparing 1, 3-propylene glycol by adopting glycerin and hydrogen
  • Technological method for preparing 1, 3-propylene glycol by adopting glycerin and hydrogen
  • Technological method for preparing 1, 3-propylene glycol by adopting glycerin and hydrogen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] one. Catalyst preparation and handling

[0032] Pour 100.0 grams of zirconium hydroxide into 50 ml of water dissolved with 2.4 grams of ammonium metatungstate, mix thoroughly, keep at 90~100°C for 20 hours, bake at 110°C to an appropriate level, extrude, dry at 110°C, and roast at 700°C After 3 hours, a tungsten-zirconium composite oxide was obtained. Take 5.0 grams of tungsten-zirconium composite oxide and immerse it in a mixed solution of 3.18ml of boric acid aqueous solution containing 8.0mg boron / ml and 1.45ml of chloroplatinic acid aqueous solution containing 70.0mg platinum / ml for 8~10 hours, dry it at 450℃ Calcined for 2-4 hours to obtain the catalyst. The mass ratio of each element in the catalyst is Pt:B:W:Zr=2:0.5:10:61.2.

[0033] A tubular fixed-bed reactor with a length of 60 cm and an inner diameter of 10 mm was used. 4.4 grams of the above-mentioned catalysts are loaded, and the particle size is 20 to 40 mesh. The catalyst was reduced in hydr...

Embodiment 2

[0045] Following the reaction of Example 1 for 100 hours, the glycerin feed mass space velocity of this reactor 2 was adjusted to 0.7h -1 , other conditions were the same as in Example 1, the reaction was continued for 100 hours, and the formation rate of 1,3-propanediol was measured in Table 2 every 25 hours during the process.

[0046] Table 2

[0047]

Embodiment 3

[0049] Reactor 2 follows embodiment 1, after embodiment 2 continuous reaction totally 200 hours, the glycerol feed quality air velocity is adjusted to 0.3h -1 , other conditions are identical with embodiment 1. The reaction was continued for 100 hours, and the formation rate of 1,3-propanediol was measured at intervals of 25 hours during the process, as shown in Table 3.

[0050] table 3

[0051]

[0052] Table 1 ~ table 3 represent, procatalyst is through embodiment 1, embodiment 2 and embodiment 3 continuous reaction totally 300 hours in this reactor 2, wherein every reaction 100 hours changes the glycerol feed mass space velocity, from each table data can It can be seen that within 300 hours of continuous reaction, under different space velocities, the formation rate of 1,3-propanediol remains stable, indicating that changing the space velocity does not affect the stability of the formation rate of 1,3-propanediol, indicating that the catalyst is stable in the continuou...

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PUM

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Abstract

The invention relates to a technological method for preparing 1, 3-propylene glycol by adopting glycerin and hydrogen. A catalyst is Pt/B2O3-WO3-ZrO2, and the mass ratio of elements of Pt, B, W and Zr is (1-4): (0.1-2): 10: (58-65); and glycerin and hydrogen are fed into a fixed bed reactor simultaneously and react at the temperature ranging from 100 DEG C to 150 DEG C under the pressure ranging from 2 MPa to 5 MPa, the resultants of reaction are subjected to gas-liquid separation, water in a liquid-phase product is separated and removed by a pervaporation membrane, a rectifying tower is used for separation, 1,3-propylene glycol, by-products containing 1,2-propylene glycol, normal propyl alcohol and isopropyl alcohol and non-converted glycerin are obtained, glycerin and a part of the by-products are circularly returned to the reactor, and the mass ratio of the circulation volume of the by-products to feeding glycerin is 0.25-1.5. According to the technological method, the reaction condition is temperate, the producing speed of 1, 3-propylene glycol is high, and 1, 3-propylene glycol can be prepared stably.

Description

technical field [0001] The invention relates to a process for preparing 1,3-propanediol by hydrogenating glycerin as a raw material. Background technique [0002] 1,3-propanediol is an important chemical raw material, which can be used as a polymer monomer to synthesize polymer materials with excellent properties. The polyester fiber propylene terephthalate ( PTT), compared with polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), has better characteristics, and has both the high performance of PET and the ease of processing of PBT, so 1,3-propanediol has broad application prospects in the production of plasticizers, detergents, preservatives, emulsifiers and other fields. [0003] At present, the preparation methods of 1,3-propanediol mainly include: ethylene oxide method, acrolein hydration method, microbial fermentation method and glycerin catalytic conversion method. Both the ethylene oxide method and the acrolein hydration method require a two-step r...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/60B01J23/652
CPCC07C29/60B01J23/6527
Inventor 陈长林管俊明杨玲
Owner NANJING UNIV OF TECH
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