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Benzoyl sulfydryl ester compound as well as preparation method and application thereof

A technology of benzoyl mercapto ester and compound, which is applied in the application of emulsion polymerization emulsifier, benzoyl mercapto ester compound and its preparation field, can solve the problems of easy bubble stability, environmental pollution, easy generation of gel, etc. Purity, high purity effect

Active Publication Date: 2014-12-10
SHANGHAI DONGSHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN101397353A provides a preparation method of polymer emulsifier for ASA, which can solve the problems of poor sizing effect, easy air bubbles and poor stability caused by adding cationic starch and small molecule emulsifier in traditional ASA emulsion
For example, under the action of high shear force, it is easy to produce gel; the freeze-thaw stability of the latex is poor; when adding pigments and other components to the latex, the emulsifier and the pigment dispersant compete at the two interfaces of the latex particle and water Adsorption, affecting rheology and stability; when preparing solid products by gel method, emulsifiers will remain in the water phase, causing environmental pollution; emulsifiers will migrate during film formation; residual emulsifiers will also cause film formation The rate is slow, reducing the water resistance of the membrane, etc.

Method used

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  • Benzoyl sulfydryl ester compound as well as preparation method and application thereof
  • Benzoyl sulfydryl ester compound as well as preparation method and application thereof
  • Benzoyl sulfydryl ester compound as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The benzoyl mercapto ester compound provided in this example is mercaptoethyl 4-p-methoxyphenyl-4-oxobutyrate, and its chemical formula is as follows.

[0036]

[0037] The preparation method of this compound is:

[0038] Add 200 parts by weight of 4-p-methoxyphenyl-4-oxobutanoic acid, 70 parts by weight of mercaptoethanol, 0.5 parts by weight of sodium hydroxide, 4 parts by weight of tin protochloride, and 0.01 parts by weight of silver powder in a four-necked flask (300 mesh), pass into nitrogen protection, reflux at 75°C for 4 hours, separate the precipitate, then add about 300 parts by weight of deionized water at 5°C and 10 parts by weight of 1N hydrochloric acid, stir for 10 minutes, and let stand for 30 minutes. And keep the solution temperature below 10°C, and white crystals are precipitated, which is mercaptoethyl 4-p-methoxyphenyl-4-oxobutanoate.

Embodiment 2

[0040] The benzoyl mercapto ester compound provided in this example is 4-mercaptopropyl 4-methoxyphenyl-4-oxobutyrate, and its chemical formula is as follows.

[0041]

[0042] The preparation method of this compound is:

[0043] Add 300 parts by weight of 4-p-methoxyphenyl-4-oxobutanoic acid, 100 parts by weight of mercaptopropanol, 1 part by weight of sodium hydroxide, 2 parts by weight of tin protochloride, 0.03 parts by weight of Silver powder (300 mesh), nitrogen protection, reflux reaction at 85°C for 3 hours, separate the precipitate, then add 300 parts by weight of deionized water at about 5°C and 10 parts by weight of 1N hydrochloric acid, stir for 10 minutes, and let stand for 30 minutes , and keep the solution temperature below 10°C, white crystals are precipitated, which is 4-mercaptopropyl 4-methoxyphenyl-4-oxobutanoate.

Embodiment 3

[0045] The benzoyl mercapto ester compound provided in this example is 4-p-methoxyphenyl-4-oxobutanoic acid-(2,2'-dimethyl)mercaptopropyl ester, and its chemical formula is as follows.

[0046]

[0047] The preparation method of this compound is:

[0048]Add 250 parts by weight of 4-p-methoxyphenyl-4-oxobutanoic acid, 85 parts by weight of (2,2'-dimethyl)-1-mercaptopropanol, 0.75 parts by weight of Sodium, 3 parts by weight of stannous chloride, 0.02 parts by weight of silver powder (300 mesh), nitrogen protection, reflux at 80 ° C for 3.5 hours, separate the precipitate, then add about 5 ° C 300 parts by weight of deionized water and 1N 10 parts by weight of hydrochloric acid, stirred for 10 minutes, allowed to stand for 30 minutes, and kept the solution temperature below 10°C, and white crystals were precipitated, namely 4-p-methoxyphenyl-4-oxobutanoic acid-(2,2'- Dimethyl) mercaptopropyl ester.

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Abstract

The invention provides a benzoyl sulfydryl ester compound and a preparation method thereof as well as an application of the compound as an emulsion polymerization emulsifier. According to the benzoyl sulfydryl ester compound and the preparation method which adopts combined catalysts, the compound as the emulsion polymerization reaction type emulsifier has a good emulsifying effect and has a molecular weight adjusting effect. The emulsifier which is few in residue in the emulsion is an ideal reaction type emulsifier and can be used for preparing high quality polymeric emulsions.

Description

technical field [0001] The invention relates to the technical field of papermaking, in particular to a benzoyl mercapto ester compound, a preparation method thereof, and an application as an emulsifier for emulsion polymerization. Background technique [0002] At present, in the field of international papermaking, papermaking sizing is gradually transitioning from acidic to neutral to alkaline. People have gradually developed disperse rosin size from the traditional saponification of rosin as a sizing agent, but it is still difficult to achieve neutral sizing. So people developed Synthetic sizing agents are reactive sizing agents such as AKD and ASA, but because synthetic sizing agents are easily hydrolyzed, and the hydrolyzed products are viscous substances, they cause serious pollution and stick to cylinders and nets. The use of suitable emulsifiers in the emulsion polymerization of the sizing agent can increase the conversion rate of the polymerization reaction and improv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/12C07C319/12C08F212/08C08F2/24
Inventor 施晓旦郭和森
Owner SHANGHAI DONGSHENG NEW MATERIALS
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