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Polyether-modified silicone phosphate ester salts are the polysiloxane polyether phosphate backbone-modified group introduced to form a new anionic surface active agent, has excellent antistatic property, wettability , smooth resistance, oxidation stability, non-volatile, non-toxic side effects such as overall performance, widely used in plastics, textile industry, cosmetics and other fields. At present, large-scale commercialization has not yet formed, the reported product is generally 40-80% solution in water, can not be used for organic systems, inorganic salt content, relative to a single species, but also did not polyether-modified silicone phosphate ester salts, and fatty alcohol ether phosphate ester salts to compare the application performance. After this hydrosilylation, phosphorylation, neutralization, concentration and other processes, a high concentration of synthetic ester salt polyether-modified silicone surfactant, find stable process control methods, in-depth exploration of the polyether-modified silicone phosphate ester salt composition and structure of the application properties of the product through the polyether-modified silicone phosphate ester salts, and fatty alcohol ether phosphate ester salts application performance comparison, a polyether-modified silicone phosphate ester salts to the application level evaluation. Papers with high hydrogen silicone oil as raw material by telomerization prepared series hydrogen silicone, and then use terminal polyoxyalkylene alkenyl ether hydrogen silicone graft modification, followed by a polyether modified silicone oil and phosphorylation reagent five phosphate phosphorus oxide reaction, and then hydrolysis, alkali neutralization, dehydration and purified to obtain a high concentration that the polyether-modified silicone phosphate ester salts. In the synthesis, the reaction by adjusting the main factors, namely to explore the optimal synthesis conditions, and to prepare the corresponding intermediates and products. Telomerization reaction preferred reaction conditions: material molar ratio MM: 202 = 0.8:1, concentrated sulfuric acid dosage is 2% of the total material, reaction temperature 60 ℃, reaction time 4h. Hydrosilylation reaction conditions more appropriate: the dropping of polyether feeding mode (method Ⅰ), Si-H and C = C molar ratio of 1: (1.05-1.1), amount of catalyst (Pt interest in) as hydrogen silicone oil quality 30ppm, the reaction temperature is 95-110 ℃, reaction time 3-4h. The phosphorylation and the hydrolysis reaction, preferably the reaction conditions are: the use of batches for feeding method of P2O5, add water method, the feed ratio of hydroxyl group: P2O5 ︰ water = (1.8 to 2.1): 1: (1 to 1.5) , reaction temperature 70 ~ 80 ℃, reaction time 3-4h, the hydrolysis temperature 70 ~ 80 ℃, hydrolysis time 2 ~ 3h, the resulting phosphate, acid phosphate content of less than 2%. Acid phosphate after hydrolysis with 50% NaOH solution and with water, toluene as a solvent, using wiped film evaporator, 85 ℃ ,0.09-0 .1 MPa concentrated under vacuum, the solid content can be up to 97% of the polyether-modified siloxane phosphate salt products. IR quantitative analysis of trace application hydrosilation reaction the Si-H bond concentration changes; after each reaction by the IR spectrum of raw materials and product comparison, clear progress of the reaction conditions and the product of the characteristic peak. Using 31P-NMR spectrum analysis of the molecular structure of the final product of information, known PESP-Na molecules does introduce a phosphate group, the product is phosphoric acid monoesters, diesters, pyrophosphate, a mixture of inorganic phosphate. In this paper, the application of product performance test series, a detailed study of the reaction product composition, allyl polyether structure, silicone / polyether weight ratio of the final product performance. The results show that the polyether-modified silicone phosphate ester salts antistatic performance by the monoester content, significantly affect the ratio of the hydrophilic group. With the monoester content increased, the proportion of hydrophilic groups increased, the product becomes good antistatic properties; smoothness by a single / double ester ratio, silicone / polyether weight ratio impact, with the polyether molecular weight decreases, the diester content increased , silicone / polyether weight ratio increased smoothness changed for the better, single / double ester ratio is far greater than the molecular weight of the polyether. Compared with alcohol ether phosphate salts, phosphate salts polyether modified siloxane good overall performance, with a low surface tension, smooth performance, low foam, heat, and good compatibility with non-polar solvents, etc., For those who have special requirements of the occasion. You can adjust the molecular structure of materials, synthesize different water / oil solubility products, expand its application in more areas.
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