Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of sulfurized alkylphenol metal salt with low free phenol content

A technology for sulfurizing alkylphenols and metal salts, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., to achieve the effects of strong adaptability, mild reaction conditions, and low cost

Active Publication Date: 2016-08-24
JINZHOU DPF TH CHEM CO LTD
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process is difficult to separate some amines with high boiling point and poor oil solubility

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Synthesis of sulfurized alkylphenate

[0028] ①In a 10L four-neck flask with stirring and water separator, add 675g (2.6mol) dodecylphenol, 120g (1.65mol) calcium hydroxide, 160g (0.55mol) stearic acid, 240g (3.85mol) Ethylene glycol and 125g (3.9mol) of sulfur, after adding 1125g of lauryl alcohol solvent, make the temperature rise from 60°C to 180°C, and react for a total of 7h; Introduce nitrogen gas from the bottom pipe to remove residual hydrogen sulfide gas, and when the temperature of the material drops to 160°C, the sulfidation / neutralization reaction ends;

[0029] ②Add 160g (0.55mol) of stearic acid, 925g of 150SN diluent oil and 330g (5.6mol) of calcium oxide into the reaction flask, control the temperature at 140°C, and feed 245g (5.55mol) of carbon dioxide at a flow rate of 0.15L / min. High alkali reaction; after 4 hours and 50 minutes, the reaction was completed, and the system was heated to 190°C under the condition of negative pressure 0.09Mpa to rem...

Embodiment 2

[0036] (1) Synthesis of intermediates

[0037] In a 1L four-neck flask with a stirrer and a water separator, add 310g (1.1mol) of stearic acid, 103g (1.0mol) of diethylenetriamine and 240g of toluene, start stirring, and heat the material to 120°C~ Reaction at 130°C for 1 hour, after reflux and dehydration, the solvent was distilled off under reduced pressure to obtain 390 g of stearic acid diethylene triamine, which was found to contain 3.211 mol of active hydrogen in total;

[0038] (2) Preparation of low free phenol sulfurized alkylphenol metal salt

[0039] In another 1L four-necked flask with a stirrer, add 450g of sulfurized alkylphenol calcium (TBN: 250mgKOH / g; free alkylphenol: 2.87% (0.05mol)), start stirring, and gradually add 15g of paraformaldehyde (0.5mol), warming up to 90°C, adding 52g of stearyldiethylenetriamine prepared in step (1), continuing to react at a constant temperature of 90°C for 8h, and under the condition of 160°C, distilling under reduced pressu...

Embodiment 3

[0041](1) Synthesis of intermediates

[0042] In a 1L four-neck flask equipped with a stirrer and a water separator, add 287g (1.07mol) of dodecenylsuccinic anhydride, gradually start stirring and heat up to 110°C, slowly add ethylene glycol through a constant pressure dropping funnel Amine 61g (1.02mol) and toluene 240g, start stirring, and heat to 120 ℃ ~ 130 ℃ for 10h, after reflux dehydration, vacuum distillation to remove the solvent, to obtain 316g of dodecenylsuccinyl ethylenediamine, after testing , the dodecenylsuccinylethylenediamide contains 1.852mol active hydrogen in total;

[0043] (2) Preparation of low free phenol sulfurized alkylphenol metal salt

[0044] In another 1L four-necked flask with a stirrer, add 450g of sulfurized alkylphenol calcium (TBN: 250mgKOH / g; free alkylphenol: 2.87% (0.05mol)), start stirring, and gradually add 15g of paraformaldehyde (0.50mol), heat up to 80°C, add 18g of dodecenylsuccinylethylenediamine prepared in step (1), continue to...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

A preparation method of a sulfurized alkyl phenate metal salt with the low free-phenol content comprises the following steps: in the presence of an organic solvent, anhydride and / or carboxylic acid and an amine compound react in the reflow state to prepare an intermediate containing at least one reactive hydrogen; the intermediate is mixed with a sulfurized alkyl phenate metal salt in which the content of free alkyl phenol is larger than or equal to 0.5%, and condensation reaction between the mixture and aldehyde under the condition of the solvent or diluent oil is carried out; water and the solvent are removed by the reduced pressure distillation or nitrogen purging mode to obtain the sulfurized alkyl phenate metal salt product with the low free-phenol content. The preparation method has the advantages that the operation method is simple and convenient, the cost is low, the reaction conditions are mild, the suitability is strong, the obtained sulfurized alkyl phenate metal salt product can serve as an additive or a basic raw material component for lubrication, the content of TPP in the sulfurized alkyl phenate metal salt is reduced, high safety and environmental friendliness are achieved, and environmental harm is low.

Description

technical field [0001] The invention belongs to the field of lubricating oil additive preparation, in particular to a preparation method of sulfurized alkylphenol metal salt with low free phenol content. Background technique [0002] Modern engine oil formulations usually contain a variety of additives. According to different functions, lubricating oil additives can be divided into ten main types, such as dispersants, viscosity index improvers, detergents, antiwear agents, antioxidants, corrosion inhibitors , emulsifier, friction modifier, extreme pressure agent and pour point depressant. [0003] Calcium sulfurized alkylphenate metal detergent is the main additive single agent for blending engine oil and marine oil. It can effectively neutralize the acidic substances produced by corrosion and oil oxidation, so as to improve the anti-oxidation and detergency of oil. When used with other additives, it shows satisfactory compatibility, good sludge, varnish and soot dispersan...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/28C07C323/20
Inventor 魏奇孙来银朱彦涛王思超
Owner JINZHOU DPF TH CHEM CO LTD