| Molecular Formula | C19H11Cl4N2O5S.Na.H2O |
| Molar Mass | 562.19 |
| Melting Point | 223 °C |
| Appearance | morphology neat |
| Physical and Chemical Properties | Chemical properties white powder. Melting point 200-205 ℃. Soluble in boiling water, tasteless. |
| Use | Use of wool fiber or its fabric infestation is caused by feeding on the worms. There are two types of feeding on the worms, one is the Lepidoptera moths and the other is the coleopteran beetle. They use keratin as food; Every year in 4-5 months in the active period, humid and hot environment is more conducive to infestation. Can be used with a variety of acid dyes, the treated fabric resistance to sunlight, washing, perspiration, rubbing and other fastness and anti cavity properties are very good. |
| Risk Codes | R20/22 - Harmful by inhalation and if swallowed. R51/53 - Toxic to aquatic organisms, may cause long-term adverse effects in the aquatic environment. |
| Safety Description | S60 - This material and its container must be disposed of as hazardous waste. S61 - Avoid release to the environment. Refer to special instructions / safety data sheets. |
| UN IDs | UN3077 9/PG 3 |
| WGK Germany | 2 |
| RTECS | DB5075000 |
Toxic to animals, with an oral LD50 of 750-1300mg/kg in rats. May cause pollution to water bodies.
1. Synthesis of 4,4 '- Dichloro-2-nitrodiphenyl ether
Add p-chlorophenol, 2,5-dichloronitrobenzene, and potassium hydroxide in a molar ratio of 1:1:1.2 to the reactor, heat to 165 ℃ under stirring, and maintain for 5 hours. After the reaction is completed, filter out potassium chloride while it is hot, wash the filter cake with benzene, and merge the benzene solution into the filtrate. Perform vacuum distillation on the combined filtrate (222 ℃, 146 ℃) × A light yellow crystal with a melting point of 75-76 ℃ was obtained, which is 4,4 '- dichloro-2-nitrodiphenyl ether.
2. Synthesis of 4,4 '- Dichloro-2-nitrodiphenylether-2' - sulfonic acid
Add the intermediate obtained above to an equal amount of sulfuric acid (96%) while stirring at room temperature, raise the temperature to 100 ℃, and dissolve completely after about 12 hours. Then, cool down with ice salt water to precipitate light yellow crystals of 4,4 '- dichloro-2-nitrodiphenylether-2' - sulfonic acid. After filtration, dissolve them in hot water and adjust the pH to 8-9 with sodium hydroxide to obtain 95% sodium salt.
3. Synthesis of 4,4 '- Dichloro-2-aminodiphenylether-2' - sulfonic acid
Dissolve the synthesized sodium salt in water, add acetic acid and iron powder (80 mesh) at 100 ℃, and keep it warm for 5 hours. After the reaction is completed, it is cooled, filtered, and washed with water. The filter cake is heated and stirred in a 5% sodium hydroxide solution, then filtered. The filter residue is washed with a small amount of water, and the filtrate is acidified with hydrochloric acid to precipitate nearly colorless crystals, which are 4,4 '- dichloro-2-aminodiphenylether-2' - sulfonic acid.
4. Synthesis of mothproof agent FF
Dissolve the synthesized crystal (3) in 0.8% sodium carbonate, add 3,4-dichlorophenyl isocyanate at 12 ℃, continue stirring at this temperature for 30 minutes, then heat up to 90 ℃ and stir for 2 hours, filter out insoluble substances, cool the filtrate to crystallize, filter and dry to obtain colorless crystals, which is the product.
| EPA chemical information | Sulcofuron-sodium (3567-25-7) |
p-chlorophenol and 2, 5-dichloronitrobenzene are used as starting materials and are prepared by the following steps. Preparation of 1.4,4 '-dichloro-2-nitrodiphenyl ether (Ⅰ) 64.3g of p-chlorophenol, 96g of 2.5-dichloronitrobenzene and 32.5g of potassium hydroxide were stirred at 160-170 ℃ for 5h. Filter while hot, filter out potassium chloride, distill the filtrate under reduced pressure, and collect 220-230 ℃(1.47kPa) fraction. After cooling, it is light yellow crystal with a melting point of 75-76.5 ℃. Preparation of 2.4,4 '-dichloro-2-nitrodiphenyl ether -2'-sulfonic acid (II) 200g of 4,4 '-dichloro-2-nitrodiphenyl ether, gradually adding 700g of 96% H2SO4 at room temperature, heating to 100 ℃, stirring for 10h. Then add it to 1.5kg of ice water to precipitate light yellow crystals. Filtered, dissolved in hot water, adjusted to be weakly alkaline with liquid alkali, precipitated odd, light yellow crystals of 4'-dichloro-2-nitro-diphenyl ether -2 '-sodium sulfonate. Preparation of 3.4,4 '-dichloro -2-amino-diphenyl ether -2'-sulfonic acid (Ⅲ) 50g of sodium 4,4 '-dichloro -2-nitro-diphenyl ether -2'-sulfonic acid is dissolved in 500ml of water, 150ml of glacial acetic acid is added in a boiling water bath under constant stirring, and 50g of iron powder is continuously added in a small amount. After that, continue heating and stirring reaction for 5h. Cool, filter out insoluble matter, wash with water. The filter cake is heated and stirred in 5% NaOH, filtered while hot, the filtrate is acidified with hydrochloric acid, and sulfamic acid crystals are precipitated. 4. Preparation of Mitine FF 4,4 '-dichloro -2-amino-diphenyl ether -2'-sulfonic acid 16.7g is dissolved in dilute sodium carbonate aqueous solution, under stirring, at a temperature of 10 ℃, and 9.4g of 4-dichlorophenyl isocyanate is added. After reacting at 10-15 ℃ for 0.5h, the reaction was continued at 90 ℃ for 2h. Filter while hot, and the filtrate cools down to get midin FF.