CN104496761A - Bisphenol A preparation method - Google Patents

Abstract

The invention relates to a bisphenol A preparation method and aims to solve the catalyst problems of desorption, low activity, too many byproducts and low conversion rate and selectivity in the prior art. The method comprises the following specific steps: mixing reaction materials phenol and acetone according to a mole ratio of 5:1, putting into a reactor containing 12-phosphotungstic acid used as a primary catalyst and mercaptoethylamine hydrochloride used as a cocatalyst, and stirring the reaction materials and the catalysts in the reactor at 75-100 DEG C for 4-6 hours to perform sufficient condensation reaction on the reaction materials; and performing reduced-pressure vacuum filtration on the reaction mixture while hot, performing vacuum concentration and dewatering on the filtrate, distilling off residual phenol and byproducts, and finally performing crystallization and purification treatment to obtain a pure product bisphenol A. According to the invention, the process is simple and adopts a reasonable reaction material ratio; the catalysts have high catalytic activity; the byproducts are reduced; the single-pass conversion and selectivity of the reaction materials are improved; and the production cost is lowered.

Description

A kind of method preparing dihydroxyphenyl propane

Technical field

The present invention relates to a kind of preparation method of organic compound, specifically a kind of production method of dihydroxyphenyl propane.

Background technology

The formal name used at school of dihydroxyphenyl propane is 2,2-biconjugate phenol propane (Bisphenol A, be called for short BPA), it is important Organic Chemicals, mainly for the production of multiple macromolecular materials such as polycarbonate, epoxy resin, polysulfone resin, polyphenylene oxide resins, also can be used on the fine chemical products such as softening agent, fire retardant, oxidation inhibitor, thermo-stabilizer, rubber antioxidant, agricultural chemicals, coating.At present, produce the method for BPA and mainly adopt Zeo-karb as catalyzer, carry out reacting using phenol and acetone as raw material and through purifying and obtaining after crystallization.Need in the process of producing BPA owing to adopting the method to adopt excessive phenol, the low conversion rate of acetone, catalyst activity is low, and work-ing life is short, and produces a large amount of by products in the process of reaction, and cause the efficiency of producing dihydroxyphenyl propane low, output is few.Therefore, a kind of new preparation method of exigence solves the problems of the technologies described above.

Summary of the invention

The present invention is just for the technical problem existed in prior art, and provide a kind of method preparing dihydroxyphenyl propane, present method easy handling, the by product of generation is less, and effectively can improve productive rate and the purity of dihydroxyphenyl propane.

To achieve these goals, the technical solution used in the present invention is, a kind of method preparing dihydroxyphenyl propane, specifically comprises the following steps:

Step one: catalyst treatment: adopt 12 phospho-wolframic acids as Primary Catalysts, mercaptoethylamine hydrochloride is promotor, and is filled in reactor after Primary Catalysts and promotor are carried out reaction treatment according to a certain amount of mixing;

Step 2: throw in reaction mass: be simultaneously throw in in reactor after 5:1 proportioning according to mol ratio by phenol and acetone;

Step 3: catalytic synthesis: on the reactor that reaction mass is housed, temperature regulator is housed, controls the temperature in reactor at 75 ~ 100 DEG C, and stirs 4 ~ 6 hours under this temperature condition, allows reaction mass fully carry out condensation reaction;

Step 4: reaction mixture filters: the reaction mixture through step 3 gained is delivered to strainer and carries out decompress filter, the water, unreacted acetone and the catalyzer that reaction are generated are separated from reaction mixture;

Step 5: crystallization: crystallization is made up of multiple crystallizer, suspension liquid bath, whizzer and adducts dissolution kettle, wherein each crystallizer is equipped with agitator, spiral coil cooling tube and chuck, containing BPA, by product and a small amount of phenol in reaction mixture after filtration after process, the BPA adducts of melting will be obtained after carrying out crystallization treatment through the reaction mixture of step 4 process;

Step 6: purify: thin-film evaporator squeezed into by the BPA adducts pump of melting, under vacuum by this adducts thermal degradation, steam most of phenol, form thick BPA, thick BPA removes residual phenol and by product from base of evaporator through being pumped in stripping tower, thus obtain sterling BPA, and infrared spectra-NMR (Nuclear Magnetic Resonance) spectrum is utilized to analyze.

Relative to prior art, originally have employed more rational reaction mass proportioning, and select mercaptoethylamine hydrochloride as promotor, substantially increase the catalytic activity of catalyzer, also reduce by product simultaneously, improve per pass conversion and the selectivity of reaction mass, reduce production cost; In addition, adopt 12 phospho-wolframic acids as catalyzer, the shortcoming such as reaction mixture aftertreatment difficulty, environmental pollution, equipment corrosion brought in producing can be avoided.

Embodiment

In order to deepen the understanding of the present invention and understanding, below the invention will be further described and introduce.

Prepare a method for dihydroxyphenyl propane, specifically comprise the following steps:

Step one: catalyst treatment: adopt 12 phospho-wolframic acids as Primary Catalysts, mercaptoethylamine hydrochloride is promotor, and is filled in reactor after Primary Catalysts and promotor are carried out reaction treatment according to a certain amount of mixing;

Step 2: throw in reaction mass: be simultaneously throw in in reactor after 5:1 proportioning according to mol ratio by phenol and acetone; Specifically phenol is put into reactor by phenol groove, acetone is put into reactor by acetone groove.

Step 3: catalytic synthesis: on the reactor that reaction mass is housed, temperature regulator is housed, controls the temperature in reactor at 75 ~ 100 DEG C, and stirs 4 ~ 6 hours under this temperature condition, allows reaction mass fully carry out condensation reaction;

Step 4: reaction mixture filters: the reaction mixture through step 3 gained is delivered to strainer and carries out decompress filter, the water, unreacted acetone and the catalyzer that reaction are generated are separated from reaction mixture;

Step 5: crystallization: crystallization is made up of multiple crystallizer, suspension liquid bath, whizzer and adducts dissolution kettle, wherein each crystallizer is equipped with agitator, spiral coil cooling tube and chuck, containing BPA, by product and a small amount of phenol in reaction mixture after filtration after process, the BPA adducts of melting will be obtained after carrying out crystallization treatment through the reaction mixture of step 4 process;

Step 6: purify: thin-film evaporator squeezed into by the BPA adducts pump of melting, under vacuum by this adducts thermal degradation, steam most of phenol, form thick BPA, thick BPA removes residual phenol and by product from base of evaporator through being pumped in stripping tower, thus obtain sterling BPA, and infrared spectra-NMR (Nuclear Magnetic Resonance) spectrum is utilized to analyze.

It should be noted that above-described embodiment, be not used for limiting protection scope of the present invention, equivalents done on the basis of technique scheme or the alternative scope all falling into the claims in the present invention and protect.

Claims (1)

1. prepare a method for dihydroxyphenyl propane, it is characterized in that: specifically comprise the following steps:

Step one: catalyst treatment: adopt 12 phospho-wolframic acids as Primary Catalysts, mercaptoethylamine hydrochloride is promotor, and is filled in reactor after Primary Catalysts and promotor are carried out reaction treatment according to a certain amount of mixing;

Step 2: throw in reaction mass: be simultaneously throw in in reactor after 5:1 proportioning according to mol ratio by phenol and acetone;

Step 3: catalytic synthesis: on the reactor that reaction mass is housed, temperature regulator is housed, controls the temperature in reactor at 75 ~ 100 DEG C, and stirs 4 ~ 6 hours under this temperature condition, allows reaction mass fully carry out condensation reaction;

Step 4: reaction mixture filters: the reaction mixture through step 3 gained is delivered to strainer and carries out decompress filter, the water, unreacted acetone and the catalyzer that reaction are generated are separated from reaction mixture;

Step 5: crystallization: crystallization is made up of multiple crystallizer, suspension liquid bath, whizzer and adducts dissolution kettle, wherein each crystallizer is equipped with agitator, spiral coil cooling tube and chuck, containing BPA, by product and a small amount of phenol in reaction mixture after filtration after process, the BPA adducts of melting will be obtained after carrying out crystallization treatment through the reaction mixture of step 4 process;

Step 6: purify: thin-film evaporator squeezed into by the BPA adducts pump of melting, under vacuum by this adducts thermal degradation, steam most of phenol, form thick BPA, thick BPA removes residual phenol and by product from base of evaporator through being pumped in stripping tower, thus obtain sterling BPA, and infrared spectra-NMR (Nuclear Magnetic Resonance) spectrum is utilized to analyze.