Tribromoneopentyl Alcohol

RX-973 Tribromoneopentyl Alcohol

Chemical Name:3-Bromo-2,2-bis(bromomethyl)propanol

Brand Name :RX-973

CAS No.: 36483-57-5&1522-92-5 

Molecular formula:C₅H₉Br₃O

Synonym:TBNPA,FR-513

Chemical Structure:

Applications :

RX-973 Tribromoneopentyl Alcohol is a reactive flameretardant containing approx. 73% aliphatic bromine. Major uses of  RX-973 are as a reactive intermediate for high molecular weight flame retardants, particularly in combination with phosphorus, and as a reactive flame retardant for polyurethanes where its high solubility in the system makes it especially useful. Its high bromine content and good compatibility in CFC - free PU systems enables high standards of fire retardancy to be reached together with good foam properties in both rigid and flexible PU.

Specifications :

Recommended Handling

All personnel handling this material must handle it as an industrial chemical, wearing protective

equipment and observing the precautions as described in the Material Safety Data Sheet (MSDS).

 

Packaging and Storage

Packed in 25kg PP Woven bags or 1MT bulk bags. Store in dry, well-ventilated area. Keep container closed. Keep away from heat, sparks and flames. Store away from incompatibles. Follow safe warehousing practices regarding palletizing, banding, shrink-wrapping and /or stacking.

Production process

A synthesis method of Tribromoneopentyl Alcohol, which is simple, mild in reaction conditions, easy to control, easy to industrial production, high in product quality, and environmentally friendly.

(1) Add pentaerythritol and reducing agent to the organic solvent and heat up until fully dissolved

(2) Add bromine dropwise in a reflux state, and after the dropwise addition, continue to reflux for 8-10 hours. During this process, bromine reacts with a reducing agent to obtain hydrogen bromide, and pentaerythritol undergoes a substitution reaction with hydrogen bromide;

(3) After the reaction is completed, distillation is carried out to 140-150 ℃, and organic solvents, unreacted hydrogen bromide, and water generated by the reaction are evaporated

(4) Cool down to 80 ℃, add catalyst to the residual liquid after distillation, introduce alcohol gas, and react for 4-6 hours

(5) After the reaction is completed, cool the above mixture to 50 ℃, then add a dispersant, and adjust pH to neutral with a 5% -10% sodium carbonate aqueous solution

(6) Add the mixed organic matter obtained above to water for crystallization, wash, dry, and slice to obtain the product

Preferably, the molar ratio of pentaerythritol to reducing agent is 1:2-4, the molar ratio of bromine to pentaerythritol is 2-4:1, the amount of catalyst added is 2-5% by mass of the residual liquid, the molar ratio of alcohol gas to pentaerythritol is 2-4:1, and the amount of dispersant added is 0.5% -1% by mass of the mixture

Preferably, the reducing agent is one or more of urea, ammonia water, or hydrazine hydrate

Preferably, the organic solvent is one or more of formic acid, acetic acid, propionic acid, benzoic acid, and boric acid

Preferably, the molar ratio of the organic solvent to pentaerythritol is 2-4:1

Preferably, the catalyst is one or more of benzenesulfonic acid, tetrabutyl titanate, tetraisopropyl titanate, and tin tetrachloride

Preferably, the dispersant is one or more of OP-10, fatty alcohol ether phosphate, phenol ether phosphate, hydroxyethyl cellulose, and sodium dodecylbenzene sulfonate

Preferably, the alcohol is one or more of isopropanol and isooctanol

Preferably, the temperature at which alcohol gas is introduced for reaction in step (4) is 100-180 ℃

Preferably, the crystallization temperature in step (6) is 5-20 ℃, and the drying temperature is 85-105 ℃

Adavantage:Using pentaerythritol, reducing agent, and bromine as the starting materials, Tribromoneopentyl Alcoholwas prepared through a two-step reaction of bromination and de esterification. A new production process was adopted, with a maximum reaction yield of over 95%, low cost, high product quality, mild reaction conditions, easy control, and environmentally friendly.

A synthesis method of Tribromoneopentyl Alcohol, comprising the following steps:

(1) Add 136g of pentaerythritol and 125g of reducing agent urea to 220g of organic solvent acetic acid, and heat up to 140 ℃ for complete dissolution

(2) In the reflux state, 320g of bromine is added dropwise. After the dropwise addition, the reflux is continued for 10 hours for insulation. During this process, bromine reacts with the reducing agent urea to obtain hydrogen bromide, and pentaerythritol undergoes a substitution reaction with hydrogen bromide

(3) After the reaction is completed, distillation is carried out to 150 ℃, and acetic acid, unreacted hydrogen bromide, and water generated by the reaction are distilled out

(4) Cool down to 80 ℃, add 8g of catalyst tetrabutyl titanate to the residual liquid after distillation, introduce 180g of isopropanol, and react for 5 hours at a temperature of 160 ℃. During the intermediate process, recover isopropanol and the generated propyl acetate

(5) After the reaction is completed, cool to 50 ℃, add 2g of dispersant fatty alcohol ether phosphate ester, stir until mixed, and then adjust pH to neutral with 5% sodium carbonate aqueous solution

(6) Add the mixed organic matter obtained above to 2000g of water for dispersion, and obtain the product through crystallization, washing, drying, and slicing. The crystallization temperature is 10 ℃ and the drying temperature is 95 ℃

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