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Biphenol compound preparation method

A biphenol and compound technology, applied in the field of preparation without using any solvent, can solve the problem of unsatisfactory effective conversion rate of raw materials, etc.

Active Publication Date: 2014-02-05
四川宝利丰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the reaction process is carried out in an autoclave, the possible reaction forms / processes of the raw materials during the reaction are more complicated, so although this method controls the reaction conditions more strictly, to reduce the formation of by-products , but the effective conversion rate of its feedstock is still unsatisfactory

Method used

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  • Biphenol compound preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 100g of 2,6-dimethylphenol into the reactor, and raise the temperature to 50°C under the protection of nitrogen. After fully melting the 2,6-dimethylphenol, add 1g of catalyst sodium hydroxide, and continue to heat up to 150°C, fully stir and mix evenly. Then stop feeding nitrogen, change to feed oxygen at a speed of 15ml / min, control the reaction temperature at 150~160°C, react for 6 hours, and the total oxygen feeding amount is 0.241mol (29.4% of the molar weight of raw materials). Stop feeding oxygen, change to nitrogen, and raise the temperature to 225~235°C to react for 2 hours. After the reaction, distill under reduced pressure of relative vacuum -0.07Mpa, collect 14g of 2,6-dimethylphenol fraction, wash and dry the crude product, and obtain the product 2,2',6,6'-tetramethyl -4,4'-biphenyldiphenol 85g white crystal, melting point 223~225℃, content 98.64%.

Embodiment 2

[0024] Add 100g of 2,6-di-tert-butylphenol into the reactor, raise the temperature to 45°C under nitrogen protection, melt the 2,6-di-tert-butylphenol, add 1.5g of catalyst calcium hydroxide, and continue to Raise the temperature to 160°C and stir well to mix evenly. Then stop feeding nitrogen, change to feed oxygen at a rate of 6.5ml / min, control the reaction temperature at 160~170°C, and react for 7 hours. . Stop feeding oxygen, change to nitrogen, heat up to 170-180°C and react for 2.6 hours. After the reaction, distill under reduced pressure at a relative vacuum of -0.08Mpa, collect 10g of 2,6-di-tert-butylphenol fraction, wash and dry the crude product to obtain the product 2,2',6,6'-tetra 89.5g of tert-butyl-4,4'-diphenol white crystals, melting point 185-187°C (standard product melting point 185-186°C), content 99.12%.

[0025] Infrared detection data of product structure: 1477.54 cm -1 , 1424.49 cm -1 (Stretching vibration of C=C benzene ring), 873.79 cm -1 (out-...

Embodiment 3

[0027] Add 100g of 2,6-di-tert-butylphenol into the reactor, raise the temperature to 45°C under nitrogen protection, melt the 2,6-di-tert-butylphenol, add 0.5g of sodium phenate catalyst, and continue to raise the temperature under nitrogen atmosphere Stir well to 170°C and mix well. Then stop feeding nitrogen, feed oxygen at a rate of 9.5ml / min, control the reaction temperature at 160-170°C, react for 5 hours, and the total oxygen feeding amount is 0.127mol (26.2% of the molar weight of raw materials). Stop feeding oxygen, change to nitrogen, and raise the temperature to 170-180°C for 3 hours. After the reaction, distill under reduced pressure at a relative vacuum of -0.09Mpa, collect 9g of 2,6-di-tert-butylphenol fraction, wash and dry the crude product to obtain the product 2,2',6,6'-tetra-tert Butyl-4,4'-diphenol white crystal 90g, melting point 185~187℃, content 99.08%.

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Abstract

The invention provides a biphenol compound preparation method. The biphenol compound preparation method is characterized in that 2, 6-dialkyl phenol is used as a raw material and is subjected to oxygen or air catalytic oxidation so as to prepare a 2, 2', 6, 6'-tetraalkyl-4, 4'- biphenol product. The reaction is carried out in the following two steps under the condition of the inexistence of a solvent: firstly smelting the 2, 6-dialkyl phenol in an inert gas environment, then mixing with hydroxide of alkali metals or alkaline-earth metals or organic salt, heating to 110-190 DEG C, and carrying oxidative coupling reaction under the condition of introducing oxygen or air; and then carrying out reduction reaction at 150-250 DEG C in an inert gas environment so as to obtain 2, 2', 6, 6'-tetraalkyl-4, 4'- biphenol product. The biphenol compound preparation method has the advantages that the yield is high, the conversion rate of the 2, 6-dialkyl phenol can reach 85-90%, and the content of the 2, 2', 6, 6'-tetraalkyl-4, 4'- biphenol product is higher than 98.5%; no solvents are used in the whole preparation process, the continuity of the production process can be realized, and the 2, 6-dialkyl phenol which is unreacted and separated out from a reaction system has good quality and can directly serve as the raw material to be recycled, so that the productivity is further increased.

Description

technical field [0001] The invention relates to a preparation method of 2,2',6,6'-tetraalkyl-4,4'-biphenyldiol, especially a preparation method without using any solvent. Background technique [0002] 2,2',6,6'-tetraalkyl-4,4'-biphenyldiol, the most commonly used is 2,2',6,6'-tetramethyl-4,4'-biphenyl Hydroquinone and 2,2',6,6'-tetra-tert-butyl-4,4'-diphenol are important raw materials for organic chemical intermediates, especially for the production of liquid crystal polymerization monomers4,4 An important intermediate of '-dihydroxybiphenyl, which itself is also a class of antioxidants. [0003] 2,2',6,6'-tetramethyl-4,4'-diphenol and 2,2',6,6'-tetra-tert-butyl-4,4'-diphenol as examples , the current relatively mature production method of 2,2',6,6'-tetraalkyl-4,4'-biphenyldiphenols is to use 2,6-dialkylphenol as raw material, complexed with copper amine The substance is used as a catalyst, and methanol is used as a solvent, and it is prepared through oxidation coupling...

Claims

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Application Information

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IPC IPC(8): C07C39/15C07C37/16
CPCY02P20/52C07C37/16C07C39/15
Inventor 李晶晶杨琴罗芩曾刚
Owner 四川宝利丰科技有限公司
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