Preparation method of 4,4-bi(2-sulfostyryl)-1,1-biphenyl

A sulfonic acid-based styrene and biphenyl technology, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of affecting the normal progress of the main reaction, affecting the purity and yield of the product, increasing the industrial operation cost, and achieving low production costs. , The effect of high product yield and reduced production cost

CN103755601AActive Publication Date: 2014-04-30HEBEI XINGYU CHEM
11 Cites 4 Cited by

Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2014-04-30

Smart Images

  • Figure 1
    Figure 1
  • Figure 2
    Figure 2
  • Figure 3
    Figure 3
Patent Text Reader

Abstract

The invention discloses a preparation method of 4,4-bi(2-sulfostyryl)-1,1-biphenyl. According to the method, solid sodium methoxide is dissolved in DMF (Dimethyl Formamide) to form a sodium methoxide solution, and the sodium methoxide solution is used for catalyzing benzyl ester to prepare CBS-X. The preparation method comprises the concrete steps of condensation reaction, distillation, and solid and liquid separation. According to the method, few side reactions are caused, the condensation reaction time is short, the preparation method is simple, the process is easy to control, the yield of a CBS-X product is larger than or equal to 98.4%, the purity is larger than or equal to 98.5%, the quality is stable, the energy consumption is low, the production cost is lowered, and the operation is safe. The preparation method is suitable for preparing the 4,4-bi(2-sulfostyryl)-1,1-biphenyl, and the 4,4-bi(2-sulfostyryl)-1,1-biphenyl is further used as a fluorescent brightener for various detergent powder, detergent paste, fancy soaps and liquid detergents.
Need to check novelty before this filing date? Find Prior Art

Description

technical field

[0001] The invention belongs to the field of chemical additives, and relates to a method for preparing a fluorescent whitening agent, in particular to a method for preparing 4,4-bis(2-sulfonic acid styryl)-1,1-biphenyl. Background technique

[0002] 4,4-bis(2-sulfonic acid styryl)-1,1-biphenyl is a fluorescent whitening agent, referred to as CBS-X, which has excellent resistance to chlorine bleaching, acid and alkali, and sunlight , whitening and brightening effect, widely used in papermaking, textile, detergent and many other fields, it is an ideal additive for light industry and daily chemical industry, especially suitable for low temperature washing and whitening, it is currently the most effective in the washing industry in the world The best fluorescent whitening agent varieties.

[0003] The Chinese invention patent application with the application number 2010106108613 discloses a "preparation method of 4,4-bis(2-sulfonic acid styryl)-1,1-biphenyl", wh...

Examples

Embodiment 1

[0019] Example 1 A kind of preparation method of 4,4-bis(2-sulfonic acid styryl)-1,1-biphenyl

[0020] Example 1 is a preparation method of 4,4-bis(2-sulfostyrene group)-1,1-biphenyl, which is carried out according to the following steps:

[0021] ⑴Condensation reaction

[0022] Dissolve solid sodium methoxide in dimethylformamide to form a sodium methoxide solution A' with a concentration of 30%; in addition, put dimethylformamide solution into the condensation kettle, and then put in methoxide with a weight ratio of 227:208 Benzyl ester and sodium aldehyde, heated up to 80°C to dissolve, kept warm for 40 minutes, cooled to 50°C, added dropwise sodium methoxide solution A' while stirring, and the time of stirring and dropping continued for 6 hours to obtain A;

[0023] ⑵ Distillation

[0024] Heat A, raise the temperature to 50°C for the first time, keep it warm for 2 hours, raise the temperature to 200°C for the second time, and obtain B in the condensation kettle;

[00...

Embodiment 2-7

[0028] Example 2-7 The preparation method of 4,4-bis(2-sulfonic acid styryl)-1,1-biphenyl

[0029] Examples 2-7 are respectively a preparation method of 4,4-bis(2-sulfonic acid styryl)-1,1-biphenyl, the preparation steps are the same as those in Example 1, and the only difference is that The control parameters in the corresponding steps are different. The specific results are shown in Table 1:

[0030] Table 1 Relevant control parameters in the preparation method of 4,4-bis(2-sulfonic acid styryl)-1,1-biphenyl

[0031]

[0032] The preparation method of Examples 2-7 is simple, the process is easy to control, the yield of the prepared CBS-X product is ≥98.4%, the purity is ≥98.5%, the production energy consumption is less, the production cost is reduced, and the operation is safe.

Embodiment 8

[0033] Example 8 The influence on the product 4,4-bis(2-sulfonic acid styryl)-1,1-biphenyl when the solvents in the sodium methoxide solution are respectively methanol and dimethylformamide

[0034] Dissolve the solid sodium methoxide in methanol to prepare a 30% sodium methoxide solution. The solution at this time is denoted as P; dissolve the sodium methoxide solid in DMF to prepare a 30% sodium methoxide solution. At this time The solution of is denoted as Q. The content of sodium methoxide contained in solutions P and Q is the same, the solvents in the sodium methoxide solution are different, and the purity, yield and quality of the CBS-X product are all different. In this embodiment, 4,4-bis(2-sulfonic acid benzene The preparation steps of vinyl)-1,1-biphenyl are the same as in Example 1, and their difference is only in the relevant control parameters in the condensation reaction and distillation process.

[0035] Table 2 Influence of different sodium methoxide solutio...