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Method of improving sulfonation reaction efficiency and production method of dispersant MF

A sulfonation reaction and sulfonation technology, applied in chemical instruments and methods, preparation of organic compounds, formation/introduction of sulfonic acid groups/dihydroxysulfonyl groups, etc., can solve problems such as residues, explosion hazards, and high investment costs. Achieve environmental protection, reduce burden and cost, and achieve high safety effects

Active Publication Date: 2017-06-09
ZHEJIANG QICAI ECO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the azeotropic agents used in this process are solvents with low flash points, which are prone to explosion hazards, and the auxiliaries used are easy to lose a lot, and some auxiliaries remain in the product, which is carcinogenic when used in clothing dyes. risks of
The third method is to carry out the sulfonation reaction in a vacuum state, and the water generated by the reaction is taken out of the system through vacuum to ensure that the sulfonation process is complete. In this method, it is difficult to completely take out the generated water due to insufficient vacuum in the production process. Affect the sodium sulfate index of the product. In order to ensure high vacuum, it is difficult for ordinary vacuum pumps to meet the requirements. Some oil pumps are needed to ensure the vacuum degree. The investment cost is high and it is easy to wear out.

Method used

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  • Method of improving sulfonation reaction efficiency and production method of dispersant MF
  • Method of improving sulfonation reaction efficiency and production method of dispersant MF
  • Method of improving sulfonation reaction efficiency and production method of dispersant MF

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Using 3000kg washing oil (the total content of methyl naphthalene and naphthalene is 31%) as the raw material, the temperature is raised to 100℃, and 2020kg of fuming sulfuric acid with a solubility of 104.5% is pumped into the reactor, and the temperature is raised to 155℃, and the reaction is 0.5 h, vacuum, the vacuum degree is 456mmHg, take the water generated during the sulfonation process out of the system, keep the vacuum reaction for 2h, adjust the vacuum degree to 152mmHg, the reaction system is blown into nitrogen, and the water that is difficult to be taken out by the subsequent vacuum is taken out by nitrogen , The flow rate of nitrogen is 4m 3 / h, the time for introducing nitrogen gas is 4h, and the sulfonation reaction ends.

[0042] After the sulfonation reaction is over, the temperature is lowered to 100°C, water is added to adjust the acidity to 14.6%, 920kg formaldehyde is added, the temperature is increased to keep the temperature at 120°C, the pressure is...

Embodiment 2

[0045] Take 3000kg methylnaphthalene as raw material, heat up to 100℃, pump 2150kg, 98% sulfuric acid into the reaction kettle, heat up to 155℃, react for 0.5h, evacuated, the vacuum degree is 456mmHg, the sulfonation process is generated Take the water out of the system, keep the vacuum for 2 hours, adjust the vacuum degree to 152mmHg, and pass nitrogen into the reaction system. The water that is difficult to be taken out by the subsequent vacuum is carried out by nitrogen. The flow rate of nitrogen is 4m 3 / h, the time for introducing nitrogen gas is 4h, and the sulfonation reaction ends.

[0046] After the sulfonation reaction is completed, the temperature is lowered to 100°C, water is added to adjust the acidity to 15.3%, 920kg formaldehyde is added, the temperature is raised to maintain the temperature at 100°C, and the normal pressure is reacted for 6 hours.

[0047] The obtained condensation material is adjusted to pH 7.0 with 30% liquid caustic so as to obtain MF slurry, whi...

Embodiment 3

[0049] Take 2000kg naphthalene as raw material, heat up to 100℃, pump 1500kg, 98% sulfuric acid into the reaction kettle, heat up to 155℃, react for 0.5h, evacuated, the vacuum degree is 456mmHg, the water generated during the sulfonation process Take out the system, keep the vacuum for 2 hours, adjust the vacuum degree to 152mmHg, and introduce nitrogen into the reaction system, and use the nitrogen to take out the water that is difficult to carry out by the subsequent vacuum. The flow rate of nitrogen is 4m 3 / h, the time for introducing nitrogen gas is 4h, and the sulfonation reaction ends.

[0050] After the sulfonation reaction is over, the temperature is lowered to 80°C and the pH is adjusted to 7.0 with 30% liquid caustic soda, and the naphthalenesulfonic acid is precipitated when the temperature is lowered, and the naphthalenesulfonic acid product is obtained by filtration. The salt content in the wastewater is 3.6%, which is compared with the traditional process The salt ...

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PUM

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Abstract

The invention discloses a method of improving the sulfonation reaction efficiency. Sulfonation is promoted by removing water generated in a sulfonation reaction. The method is characterized by comprising the step: in a sulfonation reaction process, keeping constant pressure or vacuum, and introducing gas into a reaction system, wherein water in the reaction system is taken away as gas flows out. The invention also discloses a production method of a dispersant MF. With adoption of the sulfonation method, the dispersant MF product is obtained by means of condensation and neutral reactions. In the whole process, unmanageable solid wastes are not generated, the content of sodium sulfate of the obtained product is lower than 5%, and the product can resist 150 DEG C and meets the first grade standard.

Description

Technical field [0001] The invention relates to a method capable of improving the efficiency of the sulfonation reaction and the production process of the commonly used dispersant MF. Background technique [0002] The sulfonation reaction is that hydrogen atoms in aromatic hydrocarbon compounds such as benzene molecules are replaced by sulfonic acid groups (-SO 3 H) The substituted reaction. The sulfonation reaction between sulfuric acid and fuming sulfuric acid is called liquid-phase sulfonation. Sulfuric acid acts as a sulfonating agent, solvent and dehydrating agent in the reaction system. The sulfonation reaction is a typical electrophilic substitution reaction. The reaction process with sulfuric acid as the sulfonating agent is generally considered as follows: [0003] [0004] [0005] [0006] This is the equilibrium reaction, SO 3 H + Attack the aromatic ring. The less water in the system, the SO 3 H + The higher the concentration, the easier the reaction proceeds in the...

Claims

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Application Information

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IPC IPC(8): C07B45/02B01F17/12C07C309/36C07C303/32C07C303/06C07C303/22C07C303/44C09K23/12
CPCC07B45/02C07C303/06C07C303/22C07C303/32C07C303/44C09K23/00
Inventor 张云保郭晓峰梁伟徐雷金杨建青王慧沈一鸣
Owner ZHEJIANG QICAI ECO TECH CO LTD
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