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Novel method for preparing naphthalene sodium sulfonate formaldehyde condensation compound through continuous flows

A technology of sodium naphthalene sulfonate and formaldehyde condensate, which is applied in the preparation of sulfonic acid, sulfonate, organic chemistry, etc. Solve the problems of high temperature and viscosity, reduce the amount of concentrated sulfuric acid, and have the effect of uniform and rapid reaction

Active Publication Date: 2018-12-28
江苏精禾界面科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, there are obvious disadvantages in the batch reaction synthesis of naphthalene-based sodium sulfonate formaldehyde condensate: ① high-temperature sulfonation due to excess sulfuric acid or local high temperature or uneven material mixing, side reactions of multiple sulfonation and sulfone generation are easy to occur; ② In order to fully sulfonate and reach the total acidity required by condensation, sulfuric acid is often excessive, and there is too much sulfuric acid in the condensation liquid. After neutralization by liquid caustic soda, the sodium sulfate content in the product will exceed the standard; It will lead to temperature shifting of the kettle material and cause safety accidents; or lead to local overheating or excessive aldehyde-naphthalene ratio, which will cause violent polymerization and affect product quality; Damage or even burnt; ⑤ The speed of adding alkali in the neutralization reaction is too fast, and the risk of overflow is prone to occur

Method used

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  • Novel method for preparing naphthalene sodium sulfonate formaldehyde condensation compound through continuous flows
  • Novel method for preparing naphthalene sodium sulfonate formaldehyde condensation compound through continuous flows

Examples

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Effect test

Embodiment 1

[0035] A kind of new method that continuous flow prepares naphthalene series sodium sulfonate formaldehyde condensate, the steps are as follows:

[0036] 1) Sulfonation: Add 64g refined naphthalene in stirred tank A and heat up to 85°C for melting, add 50g concentrated sulfuric acid (98%) in stirred tank B, set the temperature of the inner helical tubular reactor at 150°C, and use a push injection pump to Molten naphthalene was injected at a speed of 2mL / min and concentrated sulfuric acid at a speed of 1mL / min into an inner helical tubular reactor for reaction to synthesize a sulfonated liquid, which was collected in a stirred tank C with a temperature of 100°C, and the discharge rate was controlled to be 3mL / min. min, the sulfonated liquid stays in the reactor for 8 min.

[0037] 2) Condensation: Add an appropriate amount of water to the sulfonated solution to adjust the acidity to 18-19%, and at the same time add 32g of 37% formaldehyde solution to the stirred tank D, adjust...

Embodiment 2

[0042] A kind of new method that continuous flow prepares naphthalene series sodium sulfonate formaldehyde condensate, the steps are as follows:

[0043]1) Sulfonation: Add 64g of industrial naphthalene in stirred tank A and heat up to 85°C for melting, add 51g of concentrated sulfuric acid (98%) in stirred tank B, set the temperature of the inner helical tubular reactor at 145°C, and use a push injection pump to Molten naphthalene was injected into the internal helical tubular reactor at a speed of 1.8mL / min, and concentrated sulfuric acid was injected into an inner helical tubular reactor at a speed of 0.8mL / min to react and synthesize sulfonated liquid, which was collected in a stirred tank C with a temperature of 100°C, and the discharge speed was controlled to 2.6mL / min, the sulfonated liquid stays in the reactor for 10min.

[0044] 2) Condensation: Add an appropriate amount of water to the sulfonated solution to adjust the acidity to 19-20%, and at the same time add 30g ...

Embodiment 3

[0049] A kind of new method that continuous flow prepares naphthalene series sodium sulfonate formaldehyde condensate, the steps are as follows:

[0050] 1) Sulfonation: Add 71g of methylnaphthalene to the stirred tank A and heat up to 40°C to melt, add 52g of concentrated sulfuric acid (98%) to the stirred tank B, set the temperature of the inner helical tubular reactor at 148°C, and use a push injection pump Push molten naphthalene at a speed of 2.2mL / min and concentrated sulfuric acid at a speed of 1.1mL / min into an inner helical tubular reactor for reaction to synthesize a sulfonated liquid, which is collected in a stirred tank C with a temperature of 100°C, and the discharge speed is controlled 3.3mL / min, make the sulfonated liquid stay in the reactor for 7min.

[0051] 2) Condensation: Add an appropriate amount of water to the sulfonated solution to adjust the acidity to 18-19%. At the same time, add 28g of 37% formaldehyde solution into the stirred tank D, adjust the te...

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Abstract

The invention discloses a novel method for preparing a naphthalene sodium sulfonate formaldehyde condensation compound through continuous flows. The method comprises the following steps: putting a naphthalene compound into a stirring kettle A at a kettle temperature of 40-90 DEG C; putting concentrated sulfuric acid into a stirring kettle B; injecting into an internal spiral tube type reactor at the same time, and controlling the temperature to 140-150 DEG C to carry out a reaction so as to obtain a sulfonation liquid; putting the sulfonation liquid into a stirring kettle C, adjusting the acidity to 15-20%, putting a formaldehyde solution into a stirring kettle D, injecting into the internal spiral tube type reactor at the same time, and controlling the temperature to 105-120 DEG C to carry out a reaction so as to obtain a condensation liquid; putting the condensation liquid into a stirring kettle E, and keeping the temperature at 100 DEG C; putting a sodium hydroxide solution into a stirring kettle F, and injecting into the internal spiral tube type reactor at the same time, and controlling the temperature to 70-90 DEG C to carry out a reaction so as to obtain a neutralization product; drying the neutralization product, and evaporating off moisture, thereby obtaining a brown-yellow solid product. The novel method is safe, simple and efficient in process, and the synthesized naphthalene sodium sulfonate formaldehyde condensation compound is low in content of sodium sulfate, and good in thermal resistance stability.

Description

technical field [0001] The invention relates to the technical field of surfactant preparation, in particular to a new method for continuous flow preparation of naphthalene series sodium sulfonate formaldehyde condensate. Background technique [0002] Naphthalene sulfonic acid formaldehyde condensate is an anionic surfactant with good emulsifying, dispersing, wetting and penetrating properties, and is widely used in leather, dyes, pesticides, construction concrete and other industries. For naphthalene-based sulfonic acid-formaldehyde condensates, batch reactions are used both at home and abroad. Naphthalene or alkylnaphthalene is used as raw material. After sulfonation with a large amount of sulfuric acid, it is condensed with formaldehyde at a total acidity of 28-32%, and the final condensate Naphthalene sodium sulfonate formaldehyde condensate can be obtained by alkali neutralization. [0003] However, there are obvious disadvantages in the batch reaction synthesis of naph...

Claims

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Application Information

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IPC IPC(8): C07C309/36C07C303/22C07C303/32C07C309/35C07C303/06
CPCC07C303/06C07C303/22C07C303/32C07C309/35C07C309/36
Inventor 陆林华张小祥蔡显刚秦敦忠
Owner 江苏精禾界面科技有限公司
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