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Sulfur-containing phenolic resin and preparation method thereof

A technology of phenolic resin and alkyl phenol, applied in the field of materials, can solve the problems of unfavorable environment, bad odor, strong smell of ethanedithiol and the like

Active Publication Date: 2018-11-23
BEIJING RED AVENUE INNOVA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this patent, ethanedithiol is used as a raw material, and ethanedithiol has a strong taste, which has adverse effects on the environment during the preparation process
In addition, ethanedithiol is easy to oxidize itself into thioether, and a foul-smelling thioether by-product will be produced during the reaction, which is difficult to control

Method used

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  • Sulfur-containing phenolic resin and preparation method thereof
  • Sulfur-containing phenolic resin and preparation method thereof
  • Sulfur-containing phenolic resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Embodiment 1, p-tert-octylphenol (PTOP) contain the preparation of monothio phenolic resin

[0068] Dissolve 38.4g (0.16mol) sodium sulfide nonahydrate in 24.1g water to prepare a 20% sodium sulfide aqueous solution. Add 41.3g (0.20mol) PTOP, 20% sodium sulfide aqueous solution to the 250mL four-neck flask with temperature control device, stirring device and back distillation device, pass into the air in the nitrogen replacement reactor, heat up to make PTOP melt . At 80°C, the reaction solution was transparent and clear, and 58.4g (0.72mol) of 37% liquid formaldehyde was added dropwise, and reacted at 80°C for 4 hours after the dropwise addition. At the end of the reaction, oxalic acid was added to neutralize the pH of the reaction solution to 6.0-7.0, and then 50.0 g of solvent toluene was added for liquid separation. At 80° C., the aqueous phase of the lower layer was extracted with a peristaltic pump, and the toluene layer was washed 3 times with water. Distillat...

Embodiment 2

[0070] Embodiment 2, the preparation of PTOP containing polysulfide phenolic resin

[0071] Add 12.0g (0.3mol) of sodium hydroxide and 16.0g (0.5mol) of sulfur into a 250ml four-neck flask equipped with a temperature control device, a stirring device and a back distillation device, add 25.0g of water, install a temperature control probe, Spherical condenser, stir until dissolved, add sulfur, increase the reaction temperature to reflux, and reflux for 4 hours to obtain a dark red transparent and clear sodium polysulfide aqueous solution. Add 41.3g (0.2mol) PTOP in the 250ml four-neck flask that sodium polysulfide aqueous solution is housed, pass into the air in the nitrogen displacement reactor, heat up and make PTOP melt. At 80°C, the reaction solution was transparent and clear, and 48.6g (0.6mol) of 37% liquid formaldehyde was added dropwise, and reacted at 80°C for 4 hours after the dropwise addition. At the end of the reaction, oxalic acid was added to neutralize the pH of...

Embodiment 3～5

[0073] Embodiment 3~5, the preparation of phenol or alkylphenol containing monothio novolac resin

[0074] The preparation process of phenol or alkylphenol-containing monothio novolac resin is the same as in Example 1, only changing the type of alkylphenol.

[0075]

Example 3

Example 4

Example 5

phenol

18.8g (0.20mol)

cresol

21.6g (0.20mol)

p-tert-butylphenol (PTBP)

30.0g (0.20mol)

20% sodium sulfide nonahydrate solution

38.4g (0.16mol)

38.4g (0.16mol)

38.4g (0.16mol)

37% liquid formaldehyde

61.6g (0.76mol)

60.0g (0.74mol)

58.4g (0.72mol)

toluene

30.0g

40.0g

50.0g

Softening Point

106.3℃

96.5℃

102.4℃

Hydroxymethyl content

10.21％

9.57％

8.42％

Free phenol content

0.04％

0.01％

0.01％

mn

1105

1148

1216

mw

2352

2574

2895

Mz

3579

4159

4725

Polydispersity

2...

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PUM

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Abstract

The invention relates to sulfur-containing phenolic resin and a preparation method thereof. Phenol or alkylphenol and aldehyde, sodium sulfide or sodium polysulfide react to prepare the sulfur-containing phenolic resin. The sulfur-containing phenolic resin contains sulfur and also contains phenolic resin and hydroxymethyl structures on phenolic resin; the sulfur can be used as a sulfur donor to achieve the crosslinking effects, and can also react with metal substances; the hydroxymethyl structures in the phenolic resin can realize the self curing and can also take Diels-Alder reaction with unsaturated substances, so that the resin can be applied to the fields of rubber, encapsulation, synthetic fiber, anti-corrosion high-temperature-resistant materials, semiconductor materials and the like.

Description

technical field [0001] The invention relates to the technical field of materials, in particular to a sulfur-containing phenolic resin and a preparation method of the sulfur-containing phenolic resin. Background technique [0002] As early as 1872, the German chemist A. Baeyer first discovered that phenols and aldehydes could be condensed in the presence of acids to obtain crystalline products and amorphous brown-red resinous products that could not be handled. In 1907, American scientist L.H. Baekeland applied for a patent on "pressurization and heating" curing of phenolic resin, and established Bakelite Company on October 10, 1910. In addition, Baekeland successfully obtained the technology of applying high pressure to make phenolic prepolymerization solidify. He also clearly pointed out that whether phenolic resin has thermoplasticity depends on the amount ratio of phenol to formaldehyde and the type of catalyst used. The material is also a thermosetting resin, which can ...

Claims

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Application Information

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IPC IPC(8): C08G75/14
CPCC08G75/14
Inventor 甄博鸣阮振刚李秋荣董栋
Owner BEIJING RED AVENUE INNOVA
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