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Preparation method and application of naphthalene sulfonate-alkyl naphthalene sulfonate-formaldehyde condensate

A technology of alkylnaphthalene sulfonate and formaldehyde condensate is applied in the directions of sulfonate preparation, sulfonic acid preparation, botanical equipment and method, etc. It is difficult to realize industrialization and other problems, and achieve the effect of improving alkylation efficiency, short carbon chain and small steric hindrance

Inactive Publication Date: 2018-12-18
江苏精禾界面科技有限公司
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Problems solved by technology

[0003] But, in the existing preparation method, naphthalene alkylation, sulfonation mainly have two kinds of approaches, all there is obvious defect: 1) use alkyl alcohol as alkylation reagent, oleum as sulfonation agent and alkylation Catalyst, alkylation and sulfonation are carried out at the same time, and the end of the reaction needs to stand and stratify to separate the spent acid. For example, the Chinese patent with publication number CN107602421A discloses a preparation process of naphthalenesulfonic acid and butylnaphthalenesulfonic acid formaldehyde condensate , wherein after naphthalene and n-butanol are mixed, add dropwise the mixed acid of sulfuric acid and oleum, after the heat preservation reaction, leave it to stand layered and separate the spent acid to obtain butyl naphthalene sulfonic acid; however, this process uses a large amount of acid, not only Increase the cost of raw materials, increase the workload of acid removal, produce a large amount of acid waste water, pollute the environment, increase the step of standing and layering, and make the operation cumbersome
2) The alkylation of naphthalene and the alkylating agent is completed first, and then the alkylated naphthalene is separated for sulfonation. In this process, the alkylation reaction is reported to be a solid acid and ionic liquid catalyzed process, which can obtain relatively high selectivity and purity. However, the catalyst is easily deactivated by the influence of raw materials, and it is expensive, has high requirements for raw materials, and complicated processes, making it difficult to realize industrialization

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  • Preparation method and application of naphthalene sulfonate-alkyl naphthalene sulfonate-formaldehyde condensate
  • Preparation method and application of naphthalene sulfonate-alkyl naphthalene sulfonate-formaldehyde condensate

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preparation example Construction

[0031] A kind of preparation method of naphthalenesulfonate-alkylnaphthalenesulfonate-formaldehyde condensate, specifically comprises the steps:

[0032] (1) Alkylation reaction: Mix naphthalene, alkylating agent and sulfuric acid in a molar ratio of 1.0:0.1-2.0:0.05-0.2; then raise the temperature to 80-150°C under stirring conditions, and heat preservation reaction 4- 6h prepares the mixed solution of naphthalene and alkylnaphthalene;

[0033] (2) Sulfonation reaction: According to the molar ratio of naphthalene group and sulfuric acid is 1.0:1.0-1.3, add sulfuric acid to the mixture of above-mentioned naphthalene and alkylnaphthalene, heat up to 150-160°C under stirring condition, heat preservation reaction 3- After 5 hours, add water to adjust the acidity to 24-26%, and prepare the sulfonated liquid;

[0034] (3) Condensation reaction: reduce the temperature of the above-mentioned sulfonated liquid to 80-90°C, then add formaldehyde aqueous solution according to the molar ...

Embodiment 1

[0046] A kind of preparation method of naphthalenesulfonate-alkylnaphthalenesulfonate-formaldehyde condensate, specifically comprises the steps:

[0047] (1) Alkylation reaction: first add 64g of refined naphthalene, 6.5g of isopropanol and 2.5g of concentrated sulfuric acid with a mass concentration of 98%; then the temperature is raised to 90°C under stirring conditions, and the insulation reaction is carried out for 6h to prepare naphthalene and The mixed solution of alkylnaphthalene, the content ratio of naphthalene and isopropylnaphthalene in the mixed solution detected by high performance liquid chromatography is 80:20;

[0048] (2) Sulfonation reaction: Add 50 g of concentrated sulfuric acid with a mass concentration of 98% to the mixed solution of naphthalene and alkylnaphthalene, heat up to 160° C. under stirring conditions, keep the temperature for 5 hours, and then add water to adjust the acidity to 26%. , to prepare sulfonated liquid;

[0049] (3) Condensation rea...

Embodiment 2

[0053] A kind of preparation method of naphthalenesulfonate-alkylnaphthalenesulfonate-formaldehyde condensate, specifically comprises the steps:

[0054] (1) Alkylation reaction: first add 64g of refined naphthalene, 13g of isopropanol and 5.0g of concentrated sulfuric acid with a mass concentration of 98%; then the temperature is raised to 85°C under stirring conditions, and the insulation reaction is carried out for 4h to prepare naphthalene and alkanes The mixed solution of base naphthalene, the content ratio of naphthalene and isopropyl naphthalene in the mixed solution detected by high performance liquid chromatography is 60:40;

[0055] (2) Sulfonation reaction: Add 55 g of concentrated sulfuric acid with a mass concentration of 98% to the mixture of naphthalene and alkylnaphthalene, heat up to 155° C. under stirring, and after 4 hours of heat preservation, add water to adjust the acidity to 25%. , to prepare sulfonated liquid;

[0056] (3) Condensation reaction: reduce...

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Abstract

The invention discloses a preparation method of a naphthalene sulfonate-alkyl naphthalene sulfonate-formaldehyde condensate. The preparation method comprises the following steps: firstly enabling naphthalene and an alkylation reagent to generate a mixed solution of naphthalene and alkyl naphthalene under the catalysis of sulfuric acid; then adding sulfuric acid into the mixed solution of naphthalene and alkyl naphthalene, and performing the sulfonation reaction; and adding formaldehyde, performing the one-pot condensation, and preparing thea naphthalene sulfonate-alkyl naphthalene sulfonate-formaldehyde condensate. By adopting the preparation method, the naphthalenesulfonic acid and alkyl naphthalene sulfonate do not need to be prepared independently, and the operation is simple; the wasteacid does not need to be removed, no acidic waste water is produced, and safety and environmental protection can be realized; and the prepared naphthalene sulfonate-alkyl naphthalene sulfonate-formaldehyde condensate is used as a dispersing agent to be applied to pesticide water dispersion granules or suspension, and has higher suspension rate and better heat storage stability.

Description

technical field [0001] The invention relates to the technical field of pesticide formulation processing, and more specifically relates to a preparation method and application of a naphthalenesulfonate-alkylnaphthalenesulfonate-formaldehyde condensate. Background technique [0002] Naphthalene sulfonic acid formaldehyde condensate is an anionic surfactant with good emulsifying, dispersing, wetting and penetrating properties. It is widely used in leather, dyes, pesticides, construction concrete and other industries. Among them, sodium naphthalenesulfonate-sodium alkylnaphthalenesulfonate-formaldehyde condensate dispersants are more excellent in all aspects than single monomer naphthalenesulfonic acid or alkylnaphthalenesulfonic acid and formaldehyde condensate dispersants. performance. At present, the method for preparing sodium naphthalenesulfonate-alkylnaphthalenesulfonate-formaldehyde condensate at home and abroad mainly contains the following steps: 1) naphthalene and sul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/35C07C309/37C07C309/36A01N25/30
CPCA01N25/30C07C2/864C07C303/06C07C303/22C07C303/32C07C15/24C07C309/35C07C309/37C07C309/36
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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