Sodium 4-chloro-2-methylphenolate synthesis
- Product Name:Sodium 4-chloro-2-methylphenolate
- CAS Number:52106-86-2
- Molecular formula:C7H7ClO.Na
- Molecular Weight:165.57
1570-64-5
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Yield:52106-86-2 98%
Reaction Conditions:
with sodium monochloroacetic acid;sodium hydroxide at 100; for 1 h;Temperature;
Steps:
1.2 2. condensation reaction
Sodium chloroacetate making: in 3000L enamel in the reactor, into the chloroacetic acid 800 kg, adding water 1250L stirring to dissolve, in the 20 °C the following batch adding anhydrous sodium carbonate, and adjust the pH value to 6.5 left, about the consumption of 450 kg of sodium carbonate, sodium acetate solution to obtain qualified chlorine, then the qualified chlorine sodium acetate solution is delivered to the condensation in the process of sodium chloroacetate metering tank in standby.In 5000L enamel reaction kettle adding 860 kg of 30% sodium hydroxide solution, opening the stirring of the cresol chlorine neighbour qualified chloride to 925 kg in the reaction, the temperature of the salt forming when the temperature reaches 100 °C when, starting to drop a knotter good chloroethyl acid sodium solution, 1 hour after adding, kettle to maintain alkaline conditions, to pH 10. Reflux heat insulation 3 hours. To the circulating water cooling to 35 °C following, separate out a large amount sodium salt, then use the separation materials are solid-liquid separation, the filter cake washing twice, shall 2 a 4 chloro sodium salt wet product.3. sodium salt preparationThe 2 a 4 chloro sodium salt wet product direct drying, to obtain the content 90.2% sodium salt of 1572 kg.Through the 2 a 4 chloro sodium salt can be preparing various content of the soluble sodium salt powder, specific example as follows:80% soluble sodium salt powder: will be 1000 kg 90.2% sodium salt by adding anhydrous sodium sulfate 120 kg, and evenly mixed to obtain white 80% soluble powder product 1115 kg.56% soluble sodium salt powder: will be 1000 kg 90.2% sodium salt by adding anhydrous sodium sulfate 600 kg, and evenly mixed to obtain white 56% soluble sodium salt powder 1600 kg.4. the acidification reactionThe 2 a 4 chloro sodium salt added to the pulp in the wet product dissolved in water, and then transported to the in the acidifies the cauldron, heating 80 °C dropwise 30% salt water acidified to pH value 1.5, lowering the temperature to 40 °C following into the filter in the filtering, washing 2 times, dried to obtain content is 98% of the finished product 1235 kg.
References:
CN106365975,2017,A Location in patent:Paragraph 0030-0053