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.

Method for preparing tri(1,3-dichloro-2-propyl) phosphonate

The invention discloses a preparation method of phosphatized sol flame retardant polyurethane powder coating. According to the preparation method, non-combustible gas can be released when added phosphatized sol is combusted, so that a gas-phase barrier effect is realized; meanwhile, zinc stannate can also be used for promoting a finished product to form a stable carbon layer, so that a cooperated fireproof effect is realized; after the phosphatized sol is subjected to organic treatment, the compatibility of the phosphatized sol and polyurethane can be effectively improved, the agglomeration is reduced and the stability strength of a finished-product coated film is improved; the phosphatized sol flame retardant polyurethane powder coating does not contain a toxic plasticizer and has good safety and environmental friendliness and excellent comprehensive performance.

Preparation method of phosphatized sol flame retardant polyurethane powder coating

The invention discloses a preparation method for tris (tribromo neopentyl alcohol base) phosphate, which comprises the following steps: (1), adding tribromo neopentyl alcohol in an organic solvent at the mass ratio of 1:(1-10), and dissolving the mixture at the temperature of 1-100 DEG C under the state of stirring; (2), under the state of stirring, adding phosphorus oxychloride into the liquid reactant obtained in the step (1), as well as a first catalyst, slowly dripping a second catalyst for reaction at the temperature of 10-100 DEG C, performing insulating and reaction for 1-24 h at the temperature of 10-100 DEG C after the completion of dripping, and obtaining a product through post-processing, wherein the molar ratio of the tribromo neopentyl alcohol to the phosphorus oxychloride is 1:(1-10). The method has the advantages of simple process procedures, high product yield, good thermal stability, high content, and lower production energy consumption, greatly reduces the discharge of the three wastes, and reduces the energy consumption of product crystallization extraction and wastewater treatment cost, as well as the manufacturing cost. The generation of three wastes including waste water is avoided, the problem of environmental pollution is avoided, and the environmental protection pressure is alleviated; and the product is high in purity, low in impurity content and high in yield.

Preparation method for tris tribromo neopentyl alcohol base phosphate

The invention discloses a mesoporous molecular sieve supported composite metal oxide alcoholysis catalyst, and a preparation method of the alcoholysis catalyst. A mixed solution of alkali metal acetates, aluminium acetate, magnesium acetate, titanium acetate and rare earth metal acetates is physically adsorbed on a mesoporous molecular sieve SBA-15, and composite metal oxides are supported on the mesoporous molecular sieve SBA-15 after a calcining process. By adding the catalyst, the synthetic yield and purity of triethyl phosphate are extremely raised, and the catalyst is easy to separate and repeatedly usable.

Mesoporous molecular sieve supported composite metal oxide alcoholysis catalyst, and preparation method of alcoholysis catalyst

The invention provides a preparation method of triphenyl phosphate. Firstly, phenol is added to an organic solvent, phosphorus oxychloride is added in a dropwise mode, meanwhile, a metal catalyst is added, and after a heat preservation reaction, triphenyl phosphate is obtained through after-treatment. The preparation method is simple in process step, high in product yield and low in production energy consumption, three-waste emission is greatly reduced, production cost is reduced, the product purity is high, the impurity content is low, and the yield is high.

Preparation method of triphenyl phosphate

A preparation method of triethyl phosphate belongs to the field of chemical industry. After phosphorus oxychloride and absolute ethyl alcohol are subjected to low-pressure esterification reaction, excessive absolute ethyl alcohol and partial chlorine hydride are sequentially removed under reduced pressure, residual chlorine hydride is removed under normal pressure and rectification is carried out under reduced pressure to obtain the finished product of triethyl phosphate. With the addition of a catalyst, the temperature of esterification reaction is lowered and the reaction speed is increased, namely, the temperature is lowered to 25 to 35 DEG C from almost 50 DEG C before, and after excessive absolute ethyl alcohol is removed, ammonia is added for neutralization to remove chlorine hydride without water introduction, thus avoiding hydrolyzing triethyl phosphate; and the entire process is simple, high in yield and low in production cost.

Preparation method of triethyl phosphate

The invention relates to a preparation method of high-purity TPP (triphenyl phosphate), which is an improvement of a refining method of TPP. The preparation method comprises the following steps: in the presence of a catalyst Lewis acid, reacting phosphorus oxychloride and phenol to obtain a crude TPP product; and after dissolving in methylbenzene, carrying out acid washing, alkali washing and water washing, and distilling to obtain the TPP product, wherein after the alkali washing, adding a methanol or ethanol solution into the crude TPP product, and reacting at 20-60 DEG C for more than half an hour (the volume ratio of the crude TPP product to the methanol or ethanol solution is 1:(0.5-3)), adding deionized water to carry out water washing, and distilling out the solvent methanol or ethanol to obtain the high-purity TPP. The method can reduce the content of triphenyl phosphite in the TPP from 1000ppm to 0-2ppm.

Xiaoxin Qu

Papers

Preparation method of triethyl phosphate

Preparation method of high-purity TPP (triphenyl phosphate)