- Method for preparing tris(1,3-dichloropropyl) phosphate
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The invention discloses a method for preparing tris(1,3-dichloropropyl) phosphate. The method specifically comprises the following steps: adding phosphorus oxychloride and 1,3-dichloropropanol into areaction kettle at a time, stirring the phosphorus oxychloride and the 1,3-dichloropropanol, raising the temperature to 110 DEG, performing a reaction on the phosphorus oxychloride and the 1,3-dichloropropanol for 1-3h, raising the temperature to 180 DEG according to the 15-30-DEG C gradient, removing generated hydrogen chloride gas under a negative pressure condition and reducing the temperature,so as to obtain a crude product; washing the crude product with alkali and water in sequence and distilling, so as to obtain the tris(1,3-dichloropropyl) phosphate. Under a catalyst-free condition, the method has the advantages of being high in product purity, high in conversion rate, mild in process conditions, and simple in operation, avoiding a problem of aftertreatment of a catalyst and lowering the production cost.
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Paragraph 0014-0018
(2019/04/09)
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- Preparation method of tris(1,3-dichloropropyl) phosphonate
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The invention discloses a preparation method of tris(1,3-dichloropropyl) phosphonate. The preparation method comprises the following specific steps: (1) preparation of catalyst: preparing a solid acidcatalyst from soluble salt of metals such as Ti, Zr and Fe; and (2) preparation of tris(1,3-dichloropropyl) phosphonate: adding the solid acid catalyst and reaction materials to a reactor at one time, raising the temperature to 120-160 DEG C for reacting for 6-10 hours, simultaneously distilling off the water generated by reaction in a pressure range of -0.2 to 0 MPa, and performing alkali washing, water washing and distillation on a crude product to obtain the tris(1,3-dichloropropyl) phosphonate. The preparation method disclosed by the invention adopts a home-made catalyst and takes dichloropropanol and phosphorus pentoxide as reaction raw materials to synthesize the tris(1,3-dichloropropyl) phosphonate, the catalyst is easy to recover and has good catalytic performance, the synthetic process of the tris(1,3-dichloropropyl) phosphonate is simple in route and easy to operate, water is generated by reaction, the process is safe and environment-friendly, and industrial production is easy to realize.
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Paragraph 0017; 0018; 0019; 0020; 0021; 0022
(2019/02/06)
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- Method for preparing tri(1,3-dichloro-2-propyl) phosphonate
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The invention provides a method for preparing tri(1,3-dichloro-2-propyl) phosphonate, which relates to the technical field of a preparation method of a fire retardant. The method adopts a self-made catalyst, and uses phosphorus oxychloride and 1,3-dichloro-2-propanol as a raw material, and adopts the following steps: phosphorus oxychloride, 1,3-1,3-dichloro-2- propanol and the self-made solid acidcatalyst are added to a reaction kettle, the materials are heated to the temperature of 100-160 DEG C for 4-6 hours, the generated hydrogen chloride gas is distilled under vacuum of -0.2-0 MPa, a crude product is washed with alkali, washed with water, and is subjected to underpressure distillation to remove water. A reaction equation is shown as the specification. The raw materials of the invention are easy to obtain, the catalyst has good catalytic performance, the product has high purity, the yield is high, the reaction is mild, the operation is simple, and the product is more suitable forindustrial production.
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Paragraph 0014-0020
(2019/01/08)
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