Background and overview[1][2]
The Chinese alias of 4-hydroxybenzenesulfonic acid is p-hydroxybenzenesulfonic acid. P-Hydroxybenzenesulfonic acid can be used as an intermediate in pharmaceutical and chemical synthesis. Its commonly used salt form is sodium p-hydroxybenzenesulfonate, sodium p-hydroxybenzenesulfonate, molecular formula C6H5NaO4S, white crystal Powder, soluble in water, hot alcohol and glycerin. Sodium p-hydroxybenzene sulfonate is a very important intermediate in organic synthesis and pharmaceutical industry. Its research value and commercial value that cannot be ignored have been gradually discovered by people.
Structure
Apply[1-5]
P-Hydroxybenzene sulfonic acid can be used for resin curing and is the most important additive in the acidic tin plating process. It also has the function of acidic resin foaming and is used as an organic intermediate. Examples of its application are as follows:
1. Preparation of a new type of aromatic side chain sulfonated diamine.
Using 4,4’-diaminodiphenyl ether as raw material, it reacts with p-hydroxybenzenesulfonic acid after oxidation and bromination, and finally undergoes reduction reaction to obtain a new aromatic side chain sulfonated diamine. The hydrophilic group sulfonic acid group in the novel aromatic side chain type sulfonated diamine of the present invention is located on the side chain group. Since its spatial position is far away from the main chain, it improves the proton conduction efficiency while avoiding the impact on the main chain structure.
The new aromatic side chain sulfonated diamine can be combined with dianhydride monomers and non-sulfonated diamine monomers to prepare sulfonated polyimides. Sulfonated polyimides can be used to prepare sulfonated polyimides with good heat resistance and stability. properties, mechanical properties and proton conductivity of proton exchange membranes. New aromatic side chain sulfonated diamines have good application prospects in proton exchange membrane fuel cells.
2. Prepare a high temperature and corrosion resistant adhesive,
It includes (by mass percentage), 30% to 40% of p-hydroxybenzenesulfonic acid-nitroacetaldehyde-latex liquid; the catalyst is caustic alkali or triphenylphosphine, and the content is 1 to 2% ; Polymerization inhibitor, which is hydroquinone or hydrophenol, content is 1 to 3%; modified nano-magnesium oxide, 2 to 20%; inorganic flame retardant, which is magnesium hydroxide, aluminum hydroxide and magnesium aluminum water Talc is composed of 2:7:3 parts by mass, and the content of the inorganic flame retardant is 5% to 10%; the balance is phenolic resin.
Among them, the p-hydroxybenzenesulfonic acid-nitroacetaldehyde-latex liquid contains 20wt% p-hydroxybenzenesulfonic acid, 20wt% nitroacetaldehyde, 3wt%~5wt% carbon black, 5wt%~ 10wt% nanoscale silica powder, 5wt% ~ 10wt% nanoscale zirconium dioxide powder, 5wt% ~ 10wt% antioxidant and 1wt% ~ 2wt% dispersant, and the rest is latex liquid.
3. Prepare a high-viscosity adhesive,
It includes (by mass percentage), 30% to 40% p-hydroxybenzenesulfonic acid-nitroacetaldehyde-latex liquid; the catalyst is caustic alkali or triphenylphosphine, and the content is 1~2% ; Polymerization inhibitor, which is hydroquinone or p-phenol, content is 1~3%; fumed silica, 2~20%; tackifier, which is γ-methacryloyloxypropyltrimethyl A mixture of silane and acrylamide with a mass ratio of 10:1, with a content of 5% to 10%; the balance is phenolic resin.
Among them, the p-hydroxybenzenesulfonic acid-nitroacetaldehyde-latex liquid contains 20wt% p-hydroxybenzenesulfonic acid, 20wt% nitroacetaldehyde, 3wt%~5wt% oxidized starch, 5wt%~ 10wt% nanoscale silica powder, 5wt%~10wt% nanoscale zirconium dioxide powder, 5wt%~10wt% antioxidant and 1wt%~2wt% dispersant, and the rest is latex liquid.
4. Prepare a naphthalene-based water reducing agent,
It includes the following steps: (1) sulfonate methylnaphthalene and phenol respectively to obtain sulfonated methylnaphthalene material and p-hydroxybenzene sulfonic acid material; (2) hydrolyze the sulfonated methylnaphthalene material to obtain a total of Unreacted methylnaphthalene or its homologues are boiled off, and the remaining sulfonated methylnaphthalene material enters the reaction in step (3); (3) the sulfonated methylnaphthalene material obtained in step (2), the sulfonated methylnaphthalene material obtained in step (1) The p-hydroxybenzenesulfonic acid material and formaldehyde acidified with concentrated sulfuric acid are subjected to a condensation reaction to obtain a condensation material; (4) alkali is added to the condensation material obtained in step (3) for neutralization reaction until the pH value is 7.5~9, and the reaction is completed to obtain Naphthalene-based water reducing agent.
The above-mentioned naphthalene-based water reducing agent has excellent properties such as good adaptability to cement, good workability of concrete, strong plastic retention performance, small loss of concrete over time, and high water reduction rate; and the preparation method is simple. ��, the reaction conditions are easy to control, and it can also reduce the production cost of naphthalene series water reducing agent.
5. Encapsulating resin for semiconductor light-emitting components with high heat dissipation, involving semiconductor light-emitting component technology,
It is prepared from the following raw materials by weight: 60-90 parts of epoxy resin hard glue, 10-18 parts of artificial geranium oil, 3-10 parts of p-hydroxybenzene sulfonic acid, and 1-1-dimethylbenzylamine 3 parts, hydrogenated castor oil 1-3 parts, antimony trioxide 5-8 parts, talc 1-3 parts, quartz 2-5 parts, alumina 2-5 parts, silicon carbide 1-3 parts, synthetic nanoparticles 10-20 servings. Due to the use of epoxy resin hard glue, artificial geranium oil, p-hydroxybenzene sulfonic acid, dimethyl benzylamine, hydrogenated castor oil, antimony trioxide, talc, quartz and alumina, the encapsulating resin is encapsulated It can be quickly dried and formed, and the added synthetic nanopowder can effectively increase the strength of the packaging resin, achieve better fixing and packaging effects, enhance the heat dissipation effect of the packaging components, and reduce attenuation. effect.
Preparation [6]
Step 1: Preparation of SO3 gas. SO3 gas used in the experiment
The SO3 gas generator is generated by adding 200ml of 65% oleum, a small amount of zeolite and 20gP2O5 to the SO3 gas generator, heating it with an electric heating mantle, and the generated SO3 gas is diluted to 7% with nitrogen before entering the human body. Sulfonator performs sulfonation reaction.
Step 2: Sulfonation reaction. In the experimental kettle-type bubbling reactor, add a certain amount of phenol and a certain amount of positioning agent, and introduce diluted SO3 gas at a certain temperature (the amount of SO3 gas slightly exceeds the theoretical amount required for the reaction). Use a super thermostat to thermostat the reactor in a water bath to control the reaction temperature while stirring. As the reaction proceeds, the viscosity of the reactants gradually increases and the color gradually turns yellow.
After the reaction is completed, it is aged for a period of time. At this time, the reaction solution will be a light yellow transparent liquid. Take the liquid and conduct thin layer chromatography analysis. When the ratio of each spectrum on the thin layer chromatography does not change, stop aeration, remove the reactants, stir gently with a glass rod, and cool. At this time, crystals precipitate, perform suction filtration, and take the suction filtration. The remaining crystals are available for later use. Dissolve the crystals after suction filtration in 200 ml of glycerol aqueous solution. The dissolved solution is subjected to steam distillation. Use thin layer chromatography to analyze the distillate and stop distillation when no o-hydroxybenzenesulfonic acid precipitates.
Main reference materials
[1] CN201410336431.5 Preparation method of a new aromatic side chain sulfonated diamine
[2] CN201610533029.5 High temperature resistant and corrosion resistant adhesive
[3] CN201610533028.0 High-viscosity adhesive
[4] CN201410831025.6 Preparation method of naphthalene-based water reducing agent
[5] CN201711495661.6 Encapsulating resin for semiconductor light-emitting components with high heat dissipation
[6] Research on the synthesis process of sodium p-hydroxybenzene sulfonate
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