Polyether amine and preparation method and application thereof
A polyetheramine and polyether technology, which is applied in the field of polyetheramine of fuel detergent and its preparation, can solve the problems such as no polyetheramine, and achieve the advantages of inhibiting the formation of deposits, reducing by-products and low production cost. Effect
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[0049] According to a first aspect of the present invention, the present invention provides a method for preparing a polyetheramine comprising the steps of:
[0050] The catalyst SO 4 -2 / ZrO 2 Was added to the polyether, epichlorohydrin was added after the epoxidation reaction, to obtain a reaction solution;
[0051] The reaction solution was separated and recovered catalyst SO 4 -2 / ZrO 2 And epichlorohydrin to give chlorohydrin intermediate product;
[0052] The solid base was added to the chlorohydrin intermediate product to ring closure reaction, to give a crude epoxy-terminated polyethers;
[0053] After filtering the crude polyether epoxy group, neutralizing agent was added to the filtrate and then adsorbent is added to obtain a purified epoxy-terminated polyethers; and
[0054] The purified epoxy-terminated polyether and an organic amine and / or an inorganic ammonium amination reaction to obtain polyether amines.
[0055] First, the present invention is a polyether as...
Example Embodiment
[0077] Example 1 Solid super-acid catalyst SO 4 -2 / Zro 2 Preparation
[0078] Zrocl 2 · 8h 2 O 15 g (accurate to 0.0001 g) was dissolved in distilled water, and a saturated zirconium salt-aqueous solution was made.
[0079] Under the rapid stirring, the dripping volume fraction was 10% to 15% of the dranon ammonia regulated solutions pH to 9 to 10, and the deposition of 24 h, filtered, washed with deionized water to 0.1 mol / L of AGNO. 3 The solution was not examined without chloride ion.
[0080] Dry filter cake 12h grinding, sieve (1.05 ~ 1.5) × 10 5 NM powder, soaked with a sulfuric acid solution, filtrate the remaining solution, dry the powder, placed in a muffle furnace for 3 h, resulting in a solid super acid catalyst SO 4 -2 / Zro 2 .
Example Embodiment
[0081] Example 2 Preparation of Polyethermine
[0082] 1) epoxidation of the polyether.
[0083] 500 g of nonylphenol polyoxypropionylene ether and 2.5 g so 4 -2 / Zro 2 The catalyst was added to 1000 ml of four flasks and stirred under nitrogen gas, and then dripped to add epoxyoxropane 55.5 g, 1H was added dropwise, and the temperature was allowed to 60 ° C, and the temperature reaction was maintained 2.5 h.
[0084] After completion of the reaction, it was lowered to room temperature, and the catalyst was separated, and the epoxy chloropropane was recovered to the epoxy chloride. Under nitrogen protection, 24 g of sodium hydroxide particles were added to the middle product, and the temperature was raised to 40 ° C for 3 h, cooling to room temperature to obtain a coarse endocyclic oxygen polyether.
[0085] After filtrate the crude epoxy-based polyester, the filtrate was collected, and the neutral acid neutralization was added thereto, and then the acidic white soil was added t...
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