Purifying method of epoxypropane

A technology of propylene oxide and purification method, applied in chemical instruments and methods, inorganic chemistry, organic chemistry and other directions, can solve the problem of high energy consumption in distillation process, difficult to reduce acetaldehyde content, and no impurity content in propylene oxide is given. and other problems to achieve the effect of enhancing the adsorption performance

Active Publication Date: 2016-11-16
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] A large number of patents have disclosed the method of adopting extractive distillation to purify propylene oxide, such as: US5849938A discloses the method that uses water or propylene glycol to purify the propylene oxide that contains methyl alcohol and acetaldehyde by extractive distillation; But, this method purifies The final propylene oxide still contains more than 100ppm of acetaldehyde and methanol
[0006] CN1307168C discloses a kind of using C 7 ~C 20 Hydrocarbons, a method of purifying propylene oxide by extractive distillation; but the content of impurities in propylene oxide after extractive distillation is not given in the patent
Only by using extractive distillation method to refine the propylene oxide product, some impurities such as acetaldehyde, methanol and methyl formate can be removed, but it is difficult to reduce the acetaldehyde content in propylene oxide to below 10ppm
[0007] The following patents also disclose the purification method of propylene oxide products, especially the purification method of aldehyde impurities in the product: US 3881996 discloses a method for purifying propylene oxide by multistage distillation, which can purify aldehydes The content is less than 10ppm, but the distillation process consumes a lot of energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: Preparation of modified zeolite molecular sieve

[0032] (1) Preparation of ZSM-5 zeolite

[0033] ZSM-5 zeolite is prepared by traditional hydrothermal synthesis method: industrial aluminum sulfate, deionized water, sulfuric acid, sodium chloride, water glass and n-butylamine (NBA) solution are mixed and stirred evenly to obtain a gel, and the Al in the gel 2 o 3 : SiO 2 : Na 2 O: H 2 The molar ratio of O:NBA was 1:30:1.5:1000:10; then the gel was moved to a hydrothermal synthesis kettle with polytetrafluoroethylene, and crystallized at a temperature of 170°C for 48h. The crystallized product was filtered, fully washed, dried in air atmosphere at 110°C for 12 hours, and calcined in air atmosphere at 550°C for 3 hours to obtain nanometer ZSM-5 zeolite.

[0034] (2) Preparation of Y zeolite

[0035] Y zeolite is prepared by traditional hydrothermal synthesis method: the directing agent, water glass, deionized water, aluminum sulfate and sodium alumina...

Embodiment 2

[0044] Embodiment 2: prepare the preparation of the propylene oxide that contains aldehydes impurity

[0045] The raw material propylene, hydrogen peroxide and solvent methanol are continuously fed from bottom to top into a fixed-bed reaction device equipped with titanium silicalite molecular sieves. The raw material propylene, hydrogen peroxide and solvent methanol are prepared according to the molar ratio of 3:1:4.5, the fixed bed reaction temperature is 40°C, and the reaction pressure is 3.0MPa. The reactor outlet product contains impurities such as unreacted raw material propylene, solvent methanol, product propylene oxide and methyl formate, acetone and acetaldehyde. Above-mentioned product separates solvent methanol and unreacted raw material propylene by processes such as rectification, condensation, is after extracting rectification with water again, application gas chromatographic analysis learns that the content of acetaldehyde in the crude propylene oxide is 166ppm....

Embodiment 3

[0046] Embodiment 3: the propylene oxide that contains acetaldehyde impurity that purification embodiment 2 obtains

[0047] A method for purifying propylene oxide, comprising the following steps: 6 kinds of zeolites prepared in Example 1 are respectively placed in stainless steel tubular reactors (φ120mm × 1000mm) of 6 fixed-bed reactors, and fixed The temperature in the bed reaction device is adjusted to 30°C and the pressure is adjusted to 0.5Mpa; the propylene oxide containing acetaldehyde impurity obtained in Example 2 enters the reaction bed of the fixed bed reaction device from bottom to top in the form of liquid phase, Its airspeed LHSV is 3.0h -1 After 120 min, the sample was collected, and the content of acetaldehyde in the purified sample was analyzed by gas chromatography. The experimental results are shown in Table 1.

[0048] Table 1: Purification results of propylene oxide containing acetaldehyde impurity in liquid phase

[0049] Adsorbent

[0050] I...

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PUM

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Abstract

The invention discloses a purifying method of epoxypropane. In a fixed bed reaction device, liquid-phase epoxypropane containing aldehyde impurities enter a reaction bed layer of the fixed bed reaction device from bottom to top, a modified zealite sieve adsorbs the aldehyde impurities in epoxypropane at the temperature of 5-60 DEG C and the pressure intensity of 0.3-10.0 Mpa, and therefore purified epoxypropane is obtained; the modified zealite sieve adsorbing the aldehyde impurities recovers aldehyde substances after being purged by inert gas at high temperature so as to restore the adsorption performance. The method is a purifying method of epoxypropane containing the aldehyde impurities with granularity of 20-200 ppm; by means of the adsorption effect of the modified zealite sieve, the method can purify epoxypropane containing the aldehyde impurities with granularity of 20-200 ppm into an epoxypropane product containing aldehydes with granularity smaller than 10 ppm.

Description

technical field [0001] The invention relates to a method for purifying propylene oxide, which mainly purifies the propylene oxide containing 20-200 ppm of aldehyde impurities. Background technique [0002] Propylene oxide is the third largest propylene derivative after polypropylene and acrylonitrile. It is a very important basic organic chemical raw material. It is mainly used to produce polyether polyols, and then to produce polyurethane. Propylene oxide can also be used to prepare non-ionic surfactants, propylene alcohol, propylene glycol, and synthetic glycerin. Fine chemicals derived from propylene oxide are used in almost all industrial sectors and in everyday life. Chlorohydrin method, co-oxidation method and direct oxidation method are relatively mature propylene oxide production technologies in industry. In particular, the method of using titanium silicalite molecular sieve as a catalyst and directly oxidizing hydrogen peroxide to synthesize propylene oxide overco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/32C07D303/04C01B39/02C01B39/38C01B39/24
CPCC01B39/026C01B39/24C01B39/38C07D301/32C07D303/04
Inventor 李进刘国东
Owner CHINA CATALYST HLDG CO LTD
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