Chromite catalyst for trimerization of ethylene into 1-hexene and preparation and application thereof

A technology of chromium catalyst and hexene, applied in the field of chromous catalyst and its preparation and application, to achieve the effect of reducing operating costs

Inactive Publication Date: 2021-07-09
BEIJING CORETEAM ENG & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Chromite catalyst for trimerization of ethylene into 1-hexene and preparation and application thereof
  • Chromite catalyst for trimerization of ethylene into 1-hexene and preparation and application thereof

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Embodiment 1

[0040] 1. Preparation of chromous isooctanoate

[0041] Under anhydrous and oxygen-free conditions, chromocene is used as raw material to react with isooctanoic acid to generate chromous isooctanoate, which is heated to remove cyclopentadiene for use.

[0042] 2. Preparation of catalyst

[0043] in the N 2 Add 10 mL of dehydrated toluene, chromous isooctanoate (0.03 mmol) synthesized in Step 1, 2,5-dimethylpyrrole (29 mg), and triethylaluminum (10 mL) into a fully replaced stirred 100 mL reactor , 1,1,2,2-tetrachloroethane (7mL, 0.54mmol), react at room temperature for 10min and set aside.

[0044] 3. Trimerization of ethylene

[0045] A 500mL autoclave was heated to vacuum for 2 hours, replaced with nitrogen several times, filled with ethylene, cooled to a predetermined temperature, and dehydrated cyclohexane (200mL) and the above-mentioned catalyst were added. The oligomerization reaction was carried out at 90°C and a pressure of 5.0 MPa. After 40 minutes of reaction, th...

Embodiment 2

[0047] 1. Preparation of chromous isooctanoate

[0048] Under anhydrous and oxygen-free conditions, chromous diacetate reacts with hydrochloric acid to generate chromous chloride, and chromous chloride, sodium hydroxide, and isooctanoic acid undergo metathesis reactions to generate chromous isooctanoate.

[0049] 2. Preparation of catalyst

[0050] in the N 2 Add dehydrated toluene (10mL), chromous isooctanoate synthesized in step 1, 2,5-dimethylpyrrole (29mg), triethylaluminum (10mL) into a fully replaced stirred 100mL reactor, 1 , 1,2,2 Tetrachloroethane (0.069mmol) was reacted at room temperature for 5 minutes before use.

[0051] 3. Trimerization of ethylene

[0052] A 500mL autoclave was heated to vacuum for 2 hours, replaced with nitrogen several times, filled with ethylene, cooled to a predetermined temperature, and dehydrated cyclohexane (200mL) and the above-mentioned catalyst were added. The oligomerization reaction was carried out at 20°C and a pressure of 5.0 M...

Embodiment 3

[0054] 1. Preparation of chromous isooctanoate

[0055] Under nitrogen protection conditions, solid metal chromium reacts with 20% hydrochloric acid at a temperature of 50-80°C to synthesize chromous chloride, which undergoes metathesis reaction with sodium hydroxide and isooctanoic acid to generate isooctanoic acid Chromous.

[0056] 2. Preparation of catalyst

[0057] in the N 2 Add dehydrated toluene (10mL), chromous isooctanoate synthesized in step 1, triethylaluminum (10mL), 1,1,2,2 tetrachloroethane (0.069 mmol) were reacted at room temperature for 5 minutes for later use.

[0058] 3. Trimerization of ethylene

[0059] A 500mL autoclave was heated to vacuum for 2 hours, replaced with nitrogen several times, filled with ethylene, cooled to a predetermined temperature, and dehydrated cyclohexane (200mL) and the above-mentioned catalyst were added. The oligomerization reaction was carried out at 20°C and a pressure of 5.0 MPa. After 20 minutes of reaction, the temperat...

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Abstract

The invention provides a chromite catalyst for trimerization of ethylene into 1-hexene and preparation and application thereof, raw materials for preparing the chromite catalyst comprise chromite organic acid salt, an electron donor, 2, 5-dimethyl pyrrole and a polydentate PNP compound, and at least one of trimethyl aluminum, triethyl aluminum, triisobutyl aluminum, trioctyl aluminum, diethyl aluminum monochloride, ethyl aluminum dichloride, ethyl aluminum sesquichloride, methylaluminoxane, modified methylaluminoxane and ethyl aluminoxane. According to the chromite catalyst, a chromite source is adopted to synthesize a chromite organic metal compound, and the step of reducing trivalent chromium into chromite by aluminum alkyl is reduced by the generated catalyst, so that the active center is ensured to be + 2 valence, the loss of the catalyst is avoided, and meanwhile, the situation that the reaction selectivity is reduced and the product yield is influenced by excessive aluminum alkyl is avoided. Therefore, 1-hexene with high activity and good selectivity is developed, and the operation cost of the 1-hexene device is greatly reduced.

Description

technical field [0001] The invention relates to a catalyst system, in particular to a chromous catalyst for ethylene trimerization into 1-hexene and its preparation and application. Background technique [0002] 1-Hexene is an important comonomer of low-pressure polyethylene. The polyethylene resin prepared with 1-hexene as a comonomer has excellent tensile strength and tear strength, which can greatly improve the polyethylene resin. Quality, foreign countries such as Europe and the United States mainly use 1-hexene as a comonomer of polyethylene. [0003] In the traditional production method, the products in the ethylene non-selective oligomerization process have a Schulz-Flory distribution, and the selectivity of specific components is poor. It requires a high-energy-consuming separation process to obtain the corresponding high-purity linear α-olefins, which cannot satisfy Increasing industrial demand for specific alpha-olefins. In recent years, the research on ethylene ...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/14B01J31/24C07C2/30C07C2/32C07C2/36C07C11/107
CPCB01J31/143B01J31/2226B01J31/2409B01J2231/20B01J2531/0238B01J2531/62C07C2/30C07C2/32C07C2/36C07C2531/14C07C2531/22C07C2531/24C07C11/107Y02P20/52
Inventor 韦先庆张建辉
Owner BEIJING CORETEAM ENG & TECH
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