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Method for synthesizing 4,4-bis(chloromethyl) biphenyl
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A technology of chloromethyl and biphenyl, which is applied in 4 fields, can solve problems such as unsatisfactory effects, complex synthesis processes, and difficult reactions, and achieve high economic benefits and promotion and application value. The synthesis process is simple and easy to operate and The effect of mastering
Active Publication Date: 2012-06-13
鞍钢化学科技有限公司
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Problems solved by technology
The main problems that exist are: the content of the synthesized 4,4'-bis(chloromethyl)biphenyl product is low, and the effect is not ideal; there are too many kinds of catalysts and diluted reactants added, and the production process is complicated; During the process, it is easy to bond into agglomerates, and it is difficult to react when deposited in the lower part, which affects the quality of synthesis; the synthesis process is complicated, the operation is difficult, or the production cost is too high
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Embodiment 1
[0014] Embodiment 1: concrete production process is:
[0015] Add 25g of biphenyl, 7g of paraformaldehyde, and 200ml of cyclohexane into a three-necked flask in turn, install a stirrer, a thermometer, and a hydrogen chloride air tube, and then pass in excess hydrogen chloride gas while stirring until the solution is saturated. The reaction was continued for 15 h at a temperature of 60°C. After the reaction was finished, 470 ml of mixed solvent prepared in advance at a weight ratio of cyclohexane to benzene of 7:3 was added. And transfer it to a separatory funnel, oscillate fully, let stand to separate layers; wait for the organic layer to be washed to neutral, and naturally cool to room temperature. Then put it into an ice-water bath to cool to 15°C, and filter with suction to obtain 4,4'-bis(chloromethyl)biphenyl crude product with a content of 80%.
[0016] Then, according to the weight of the 4,4'-bis(chloromethyl)biphenyl crude product, a mixed solvent of cyclohexane and...
Embodiment 2
[0017] Embodiment 2: the specific production process is:
[0018] Add 50g of biphenyl, 20g of paraformaldehyde, and 300ml of cyclohexane into a three-necked flask in turn, install a stirrer, a thermometer, and a hydrogen chloride air tube, and then pass in excess hydrogen chloride gas while stirring until the solution is saturated. The reaction was continued for 6 h at a temperature of 35°C. After the reaction is finished, add 740 ml of mixed solvent prepared in advance according to the weight ratio of cyclohexane and benzene at a ratio of 6:4. And transfer it to a separatory funnel, oscillate fully, let stand to separate layers; wait for the organic layer to be washed to neutral, and naturally cool to room temperature. Then put it into an ice-water bath to cool to 7°C, and filter with suction to obtain 4,4'-bis(chloromethyl)biphenyl crude product with a content of 80%.
[0019] Then, according to the weight of the 4,4'-bis(chloromethyl)biphenyl crude product, a mixed solven...
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Abstract
The invention provides a method for synthesizing 4,4-bis(chloromethyl) biphenyl. The method comprises the following steps of: continuously reacting biphenyl, paraformaldehyde and cyclohexane, which serve as raw materials, at a temperature of between 30 and 60 DEG C for 5 to 16 hours in the presence of excessive hydrogen chloride serving as a catalyst in cyclohexane and benzene mixed solvent serving as a dilution reaction medium to synthesize the coarse product of the 4,4-bis(chloromethyl) biphenyl; and obtaining the 4,4-bis(chloromethyl) biphenyl product containing over 95 percent of 4,4-bis(chloromethyl) biphenyl by recrystallizing the synthesized coarse product of the 4,4-bis(chloromethyl) biphenyl in the mixed solvent serving as a medium. The method has the advantages of reasonable composition, scientific ratio, simple and convenient synthetic process, convenient operation and control, high purity of the synthesized 4,4-bis(chloromethyl) biphenyl, over 50 percent yield and extremely high economic benefits and popularization and application values.
Description
technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a preparation method of 4,4'-bis(chloromethyl)biphenyl. Background technique [0002] 4,4'-bis(chloromethyl)biphenyl (BCMB) is an important organic synthesis intermediate, the main raw material for the synthesis of high-efficiency fluorescent whitening agent bis-stilbene CBS, and also the synthetic pharmaceutical intermediate dimethylol An important raw material for biphenyls. The CBS series fluorescent whitening agent has excellent properties such as light resistance, chlorine bleaching resistance, acid and alkali resistance and good whitening effect, so it is widely used in natural and artificial fibers and plastics such as cotton, polyvinyl chloride, polypropylene=polystyrene, etc. Whitening, the effect of whitening and brightening is very obvious. Although there are a few domestic companies that can produce bis-stilbene CBS, its quantity and quality are far from m...
Claims
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Application Information
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