A method for improving the efficiency of sulfonation reaction and the production method of dispersant mf

A production method and dispersant 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, large additives, etc., to achieve Contribute to environmental protection, reduce burden and cost, and reduce the effect of consumption

Active Publication Date: 2021-06-01
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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  • A method for improving the efficiency of sulfonation reaction and the production method of dispersant mf
  • A method for improving the efficiency of sulfonation reaction and the production method of dispersant mf
  • A method for improving the efficiency of sulfonation reaction and the production method of dispersant mf

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]The raw material was raised to 100 ° C with 3000 kg of wash oil (methyl naphthalene and naphthalene), and the pump was raised to 100 ° C, and the pump was pumped into the reactor, and the temperature was 105 ° C, and the reaction was 0.5 h, the vacuum, the vacuum is 456mmHg, the water belt in the sulfonation process is used to maintain a vacuum reaction for 2 h, and the regulatory vacuum is 152 mmHg. The reaction system is introduced into nitrogen, and the subsequent vacuum is difficult to bring out by nitrogen. , The flow rate of nitrogen is 4m3 / h, the time in which nitrogen is introduced is 4 h, and the sulfonation reaction is completed.

[0042]After the sulfonation reaction, the acidity was cooled to 100 ° C, and the acid was adjusted to 14.6%, and the formaldehyde was 920 kg, and the temperature was 120 ° C, the pressure was 0.2 MPa, and the reaction was 4 h.

[0043]The resulting condensation material was adjacent to 7.2 by 30%, and the MF slurry was dried to dry the MF produ...

Embodiment 2

[0045]With 3000 kg of methyl naphthalene as raw materials, 1050 kg, 98% sulfuric acid were raised to the reactor with a pump, and the temperature was 10.5 h, the vacuum was 456 mmHg, and the sulfonation process was generated. The water belt out of the system, maintains a vacuum reaction for 2 h, the regulatory vacuum is 152 mmHg, the reaction system is introduced into nitrogen, and the water that is difficult to bring out of the subsequent vacuum to the water, and the flow rate of nitrogen is 4m.3 / h, the time in which nitrogen is introduced is 4 h, and the sulfonation reaction is completed.

[0046]After the sulfonation reaction, the acidity was cooled to 100 ° C, and the acid was adjusted to 15.3%, add formaldehyde 920 kg, and the temperature was allowed to maintain 100 ° C, atmospheric pressure, reaction for 6 h.

[0047]The resulting condensation material was adjacent to 7.0 by 30%, and the MF slurry was obtained, and the MF product was dried. The product had a sodium sulfate content ...

Embodiment 3

[0049]With 2000kg naphthalene as raw material, 10,000 kg, 98% sulfuric acid was raised to 100 ° C, and the pump was pumped into the reactor, and the temperature was raised to 155 ° C, the reaction was 0.5h, the vacuum was 456 mmHg, and the water generated by the sulfonation process With the system, maintain a vacuum reaction for 2 h, the regulated vacuum is 152 mmHg, the reaction system is introduced into nitrogen, and the flow rate of the subsequent vacuum is difficult to bring out by nitrogen, and the flow rate of nitrogen is 4m.3 / h, the time in which nitrogen is introduced is 4 h, and the sulfonation reaction is completed.

[0050]After the sulfonation reaction, the temperature dropped to 80 ° C for 30% liquid base tuning pH of 7.0, and the precipitation of naphthalenesulfonate was precipitated, and the salt content was 3.6% in wastewater, compared to conventional process wastewater. The salt content is reduced by more than 80%. At the same time, the amount of sulfuric acid is also...

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Abstract

The invention discloses a method for improving the efficiency of sulfonation reaction, which promotes sulfonation by removing water produced in the sulfonation reaction process, and is characterized in that: during the sulfonation reaction process, normal pressure or vacuum is maintained, and the reaction system is passed Into the gas, with the outflow of gas, the water in the reaction system is taken out. The invention also discloses a production method of the dispersant MF, which uses the above-mentioned sulfonation method to obtain the dispersant MF product through condensation and neutralization reactions. The whole process does not produce difficult solid waste, the sodium sulfate content of the obtained product is less than 5%, and the heat resistance is 150°C, which meets the first-grade product standard.

Description

Technical field[0001]The present invention relates to a method capable of improving a sulfonated reaction efficiency, and a production process of commonly dispersant MF.Background technique[0002]The sulfonation reaction is a sulfonic acid group in a sulfuric acid molecule in an aromatic hydrocarbon compound such as a benzene molecule (-SO3H) The replaced reaction. Sulfonation reaction for sulfuric acid and fumeulfuric acid is referred to as liquid phase sulfonation. The effect of sulfurizers, solvent, and dehydration in the reaction system. The sulfonation reaction is a typical electrophilic substitution reaction, and the reaction process of sulfuric acid is a sulfonating agent is generally considered as follows:[0003][0004][0005][0006]This is a balance reaction, so3Hide+Attack the aromatic ring. The less water in the system, SO3Hide+The higher the concentration, the more the reaction is easier to facilitate the direction. When concentrated sulfuric acid is used as a sulfonating age...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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