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Supported Catalyst for Synthesis of Low Molecular Weight Polyethylene Oxide and Its Preparation and Application

A supported catalyst and polyethylene oxide technology, which is applied in the field of supported catalysts and preparations for the synthesis of low molecular weight polyethylene oxide, can solve the problems of not being able to use PEO, achieve low cost, reduce fluctuations, and broad market prospects

Active Publication Date: 2018-11-27
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst carrier used in this patent has fewer active sites, and the ratio of various substances in the reaction process makes the molecular weight range of the PEO prepared by the patented method wider, and the molecular weight distribution range of the PEO obtained is 60. 10,000 to 1.6 million, cannot be used to synthesize lower molecular weight PEO

Method used

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  • Supported Catalyst for Synthesis of Low Molecular Weight Polyethylene Oxide and Its Preparation and Application
  • Supported Catalyst for Synthesis of Low Molecular Weight Polyethylene Oxide and Its Preparation and Application
  • Supported Catalyst for Synthesis of Low Molecular Weight Polyethylene Oxide and Its Preparation and Application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A kind of preparation method for the supported catalyst of synthesizing low molecular weight polyoxyethylene comprises the following steps:

[0041] (1) Pretreatment of nanomaterials

[0042] A certain amount of hydrophilic silica was treated at 50°C for 6 hours.

[0043] (2) Supporting of catalyst

[0044] Weigh 5g of the above-mentioned treated hydrophilic silica and add it into a 1L reaction bottle, then slowly add 5.0g of metallic calcium (purity>99.5%) into 200mL of industrial grade liquid ammonia at -40°C to generate calcium Ammonium complex, after the reaction is complete, add the modifying agent that is dissolved in 300mL n-heptane by acetonitrile, propylene oxide (the molar ratio with the calcium element in the calcium ammonium complex is respectively 0.5 and 1), fully After the reaction, the residual liquid ammonia was volatilized at room temperature, and finally the temperature was raised to 60°C for aging. After condensing and refluxing for 1 hour, a slurr...

Embodiment 2

[0048] (1) Pretreatment of nanomaterials

[0049] Except that the calcining temperature of a certain amount of hydrophilic silica was changed to 300° C., other operations were the same as in Example 1.

[0050] (2) Supporting of catalyst

[0051] The loading preparation process is the same as in Example 1.

[0052] (3) Polymerization of ethylene oxide

[0053] The reactor used for slurry polymerization is a 10L magnetically coupled reactor with stirring, which is fed in a batch reaction mode. First, the supported catalyst prepared in step (2) was added in one go, and then 2000 mL of n-heptane and 800 g of ethylene oxide were added respectively. Wherein, the polymerization reaction is carried out at 5° C. to 25° C. for 15 hours to obtain a polyethylene oxide product. The polyethylene oxide prepared by the supported catalyst is all white powder particles, and the polymerization results are shown in Table 1.

Embodiment 3

[0055] (1) Pretreatment of nanomaterials

[0056] Except that the calcining temperature of a certain amount of hydrophilic silica was changed to 600° C., other operations were the same as in Example 1.

[0057] (2) Supporting of catalyst

[0058] The loading preparation process is the same as in Example 1.

[0059] (3) Polymerization of ethylene oxide

[0060] The reactor used for slurry polymerization is a 10L magnetically coupled reactor with stirring, which is fed in a batch reaction mode. First, the supported catalyst prepared in step (2) was added in one go, and then 2000 mL of n-heptane and 800 g of ethylene oxide were added respectively. Wherein, the polymerization reaction is carried out at 5° C. to 25° C. for 13 hours to obtain a polyethylene oxide product. The polyethylene oxide prepared by the supported catalyst is all white powder particles, and the polymerization results are shown in Table 1.

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Abstract

The invention relates to a supported catalyst for synthesizing a low molecular weight polyethylene oxide and preparation and application thereof. The catalyst comprises a calcium ammonium alkoxide compound, a catalyst support, a catalyst promoter and an inert solvent. The mole ratio of the catalyst promoter to calcium in the calcium ammonium alkoxide is (0.4-1.0):1, the mass ratio of the catalyst support to the calcium in the calcium ammonium alkoxide is (0.1-3):1, and the mass ratio of the inert solvent to the calcium ammonium alkoxide compound is (30-100):1. The preparation method comprises the steps that 1, calcium metal is added into liquid ammonia under the inert gas atmosphere; 2, an insert solvent containing an organic epoxide and the catalyst promoter organic nitrile is added with stirring; 3, the temperature is increased to normal temperature, and the liquid ammonia volatilizes; 4, the temperature is increased to carry out aging treatment on the system, and the catalyst promoter is added before any step. Compared with the prior art, the supported catalyst has the advantages that the support cost is low, catalyst particles are uniform and the activity is high, and the 100000-590000 molecular weight-level polyethylene oxide can be stably and efficiently prepared.

Description

technical field [0001] The invention relates to a preparation of a supported catalyst and a preparation method thereof, in particular to a supported catalyst for synthesizing low-molecular-weight polyethylene oxide, a preparation method and an application thereof. Background technique [0002] Polyethylene oxide is a non-ionic polymer formed by ring-opening polymerization of ethylene oxide. It has a series of excellent properties such as water solubility, thermoplasticity, and oxidative degradation. It is an environmentally friendly material. The use of polyethylene oxide is closely related to molecular weight. Among them, polyethylene oxide with low relative molecular weight (generally under 1 million molecular weight) has good water absorption, slow release, lubrication and dispersion, and is widely used in agriculture, textile, medicine, daily chemical industry Supplies and municipal engineering and other fields have a wide range of applications. [0003] The key to the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/12
CPCC08G65/12C08G2650/24
Inventor 乔新峰孔猛刘婷婷康必显罗勇
Owner SHANGHAI RES INST OF CHEM IND
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