Propylene chloride epoxidation process in the presence of hydrogen and oxygen

A technology of epoxidation and chloropropene, applied in chemical instruments and methods, organic chemistry, molecular sieve catalysts, etc., can solve problems such as environmental hazards, short life, and equipment corrosion

Active Publication Date: 2012-07-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems of this process are: serious equipment corrosion, high production energy consumption, high chlorine consumption, many by-products, a large amount of waste water containing calcium chloride and organic chloride, which seriously endangers the environment, and the investment in waste water treatment accounts for the total About 20% of the investment
However, the process flow of the propylene alcohol method is longer, and the corrosion of the equipment is still very serious. The catalyst is expensive and has a short life, which increases the production cost to a certain extent. The amount is still relatively large, and the investment in equipment maintenance and three waste treatment is still relatively large
[0004] It can be seen that the above methods have limitations, and due to environmental protection issues, developed countries and regions such as the United States and Western Europe no longer allow new plants to produce epichlorohydrin using the propylene chloride method or the allyl alcohol method.

Method used

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  • Propylene chloride epoxidation process in the presence of hydrogen and oxygen
  • Propylene chloride epoxidation process in the presence of hydrogen and oxygen
  • Propylene chloride epoxidation process in the presence of hydrogen and oxygen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069]Get 20 grams of titanium-silicon molecular sieve TS-1, concentration is 0.01g / ml (as palladium atom) ammonium nitrate palladium complex solution and appropriate amount of hydrazine hydrate and cetyltrimethylammonium bromide are added to tetrapropyl Aqueous solution of ammonium hydroxide (mass percentage concentration 10%) stirs and mixes evenly, wherein titanium silicon molecular sieve (gram): hexadecyltrimethylammonium bromide (mole): tetrapropyl ammonium hydroxide (mole): hydrated Hydrazine (mol): ammonium nitrate palladium complex (g, calculated as palladium): water (mol) = 100: 0.005: 0.5: 3.0: 2.0: 1000. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 150°C and autogenous pressure for 48 hours, filter the resultant, wash with water, dry it naturally, and continue drying at 180°C for 3 hours to obtain micropores containing precious metals Titanium silicon material A. After characterization, its composition can b...

Embodiment 2

[0071] Get 20 grams of titanium-silicon molecular sieve TS-1, a palladium chloride solution with a concentration of 0.01 g / ml (in terms of palladium atoms), and an appropriate amount of hydrazine hydrochloride and polypropylene to join in an aqueous solution of sodium hydroxide (mass percentage concentration 15%) and stir Mix well, wherein titanium silicon molecular sieve (gram): polypropylene (mol): sodium hydroxide (mol): hydrazine hydrochloride (mol): palladium chloride (gram, in palladium): water (mol) = 100: 0.9: 1.8:0.15:0.1:4600. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 180°C and autogenous pressure for 24 hours, filter the resultant, wash with water, dry it naturally, and continue drying at 110°C for 3 hours to obtain micropores containing precious metals. Titanium silicon material B. After characterization, its composition can be expressed as 8TiO in the form of oxides 2 100SiO2 2 ·0.006PdO·0.008Pd, the ...

Embodiment 3

[0073] Tetraethyl orthosilicate, tetrabutyl titanate, palladium acetate solution and Tween 80 with a concentration of 0.01 g / ml (in terms of palladium atoms) were added to the aqueous solution of tetrapropylammonium hydroxide and butylenediamine (mass The percentage concentration is 10%) and stir and mix evenly, wherein the molar composition silicon source: titanium source: tetrapropylammonium hydroxide: butylenediamine: palladium source: protective agent: water = 100: 0.03: 0.5: 0.1: 0.05: 0.02:550, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then put it into a sealed reactor, hydrothermally treat it at a temperature of 120°C and autogenous pressure for 120 hours, take out the resultant, filter it, dry it, and roast it to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the above remaining filtrate, add an appropriate amount of hydrazine hydrate, and then conduct a hy...

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Abstract

The invention discloses a method for preparing epichlorohydrin by the epoxidation of chloropropene by means of catalyzing, which is characterized in that under the conditions of temperature of 0 DEG C to 180 DEG C and pressure of 0.1 MPa to 3.0 MPa, chloropropene, oxygen, hydrogen, diluents, a solvent and a catalyst are mixed and contacted for reaction; the mole ratio of the chloropropene, the oxygen, the hydrogen, the diluents, the solvent and the catalyst is 1: (0.1 to 10): (0.1 to 10): (0 to 100); the mass ratio of the chloropropene and the catalyst is (0.1 to 50):1; the mass ratio of the solvent and the catalyst is (20 to 1000):1; the catalyst refers to a cellular titanium silicon material or a composite containing the cellular titanium silicon material; the composition of the cellular titanium silicon material expressed in the manner of oxides is xTiO2 question mark 100SiO2 question mark yEm question mark On question mark zE, wherein, the value of X is between 0.001 and 50.0; the value of (y plus z) is between 0.005 and 20.0 and y divided by z is less than 1; E represents one or more noble metals selected out of Ru, Rh, Pd, Re, Os, Ir, Pt and Au; m and n are numbers meeting the need of E at oxidation state; and the grains of the material are partially hollow or completely hollow. The method obviously promotes the transformation rate of chloropropene and has high selectivity and hydrogen effective utilization rate and long running period.

Description

technical field [0001] The present invention relates to the method for producing epichlorohydrin, more specifically the present invention relates to a kind of method for producing epichlorohydrin by epoxidation of propylene chloride. Background technique [0002] Epichlorohydrin (Epichlorohydrin, abbreviated as ECH), also known as 1-chloro-2,3-epoxypropane, commonly known as epichlorohydrin. There are epoxy groups and active chlorine in the ECH molecule, which is chemically active. The epoxy resin prepared from ECH has the characteristics of strong adhesion, corrosion resistance to chemical media, low shrinkage, good chemical stability, and high impact strength; synthetic glycerin obtained by hydrolysis of ECH is widely used in alkyd In industries such as resin, medicine, tobacco, food and explosives; chlorohydrin rubber produced by ECH homopolymerization or dimerization and trimerization with ethylene oxide and propylene oxide, has heat resistance, oil resistance, ozone re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/04C07D303/08B01J29/89
Inventor 林民史春风朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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