A kind of naphthalene series powder superplasticizer and preparation method thereof
A technology of naphthalene-based powder and water reducer, which is applied in the field of naphthalene-based powder water reducer and its preparation, which can solve the problems of powder products such as easy moisture absorption and naphthalene vapor emission, shorten production time, reduce tail gas emissions, and improve sulfonation conversion rate effect
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Embodiment 1
[0028] 1) Sulfonation: add 100 parts of industrial naphthalene to a closed reaction kettle A with a cooling reflux device on the upper part and a steam heating pipe on the lower part, heat up to 130-140 ° C, add 120 parts of concentrated sulfuric acid dropwise and add in 0.5 The dropwise addition is completed within h, and after the addition is completed, continue to heat up to 160°C to start the sulfonation reaction. After sulfonation for 1 hour, add 20 parts of methyl acetate, and continue the sulfonation for 2 hours;
[0029] The added ester compound is hydrolyzed under acidic conditions. The hydrolysis reaction will consume a certain amount of water, which will promote the sulfonation reaction to the right and increase the sulfonation conversion rate of naphthalene. However, the organic solvent for hydrolysis has a low boiling point and is easy to dissolve at high temperature. The volatilization follows the naphthalene vapor into the cooling reflux device on the upper part ...
Embodiment 2
[0037] 1) Sulfonation: add 110 parts of industrial naphthalene to a closed reaction kettle A with a cooling reflux device on the upper part and a steam heating pipe on the lower part, heat up to 130-140 °C, add 120-140 parts of concentrated sulfuric acid dropwise and The dropwise addition is completed within 0.5h. After the addition, continue to heat up to 160°C to start the sulfonation reaction. After sulfonation for 1 hour, add 30 parts of butyl formate and continue the sulfonation for 2 hours; esters are hydrolyzed under acidic conditions to promote the sulfonation of naphthalene. Transformation, the hydrolyzate can be recycled with the naphthalene vapor through the cooling reflux device, and the above-mentioned cycle and recovery steps of the ester hydrolyzate can further increase the sulfonation rate and make the reaction more complete;
[0038] 2) Hydrolysis: After the sulfonation reaction is completed, the temperature is lowered to 120-125°C, and 30-40 parts of water are...
Embodiment 3
[0045] 1) Sulfonation: Add 120 parts of industrial naphthalene to the closed reaction kettle A with a cooling reflux device installed on the upper part and a steam heating pipeline connected to the lower part, heat up to 130-140 ° C, add 140 parts of concentrated sulfuric acid dropwise and add 140 parts of concentrated sulfuric acid at 0.5 The dropwise addition is completed within h, and after the addition, continue to heat up to 160°C to start the sulfonation reaction. After sulfonation for 1 hour, add 30 parts of ethyl acetate and continue the sulfonation for 2 hours; esters are hydrolyzed under acidic conditions to promote the sulfonation conversion of naphthalene. The hydrolyzate can be recycled along with the naphthalene vapor through the cooling reflux device, and the sulfonation rate can be further improved through the above-mentioned cycle and recovery steps of the ester hydrolyzate, making the reaction more complete;
[0046] 2) Hydrolysis: After the sulfonation reacti...
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