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A comb-type multi-hydrophilic chain rosin block polyether sulfonate and its preparation method

A technology of polyether sulfonate and block polyether, applied in chemical instruments and methods, transportation and packaging, dissolution, etc., can solve problems such as deep color, low esterification rate, and low sulfonation degree of products, and achieve color Shallow, high sulfonation rate, good dispersion stability

Active Publication Date: 2020-06-12
INST OF CHEM ENG GUANGDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, although the one-pot method is simple to operate and can easily prepare surfactant products, the method has a low esterification rate and needs to use concentrated sulfuric acid or chlorosulfonic acid as a sulfonating agent, which easily leads to a low degree of sulfonation of the product , deep color

Method used

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  • A comb-type multi-hydrophilic chain rosin block polyether sulfonate and its preparation method
  • A comb-type multi-hydrophilic chain rosin block polyether sulfonate and its preparation method
  • A comb-type multi-hydrophilic chain rosin block polyether sulfonate and its preparation method

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preparation example Construction

[0035] The preparation method of the comb-shaped multi-hydrophilic chain rosin block polyether sulfonate includes the following steps:

[0036] 1) Synthesis of aconitic acid-modified rosin: melt the rosin, add aconitic acid, and fully react to obtain aconitic acid-modified rosin;

[0037] 2) Synthesis of rosin block polyether: mix aconitic acid-modified rosin and catalyst, add propylene oxide, fully react and age, then add ethylene oxide, fully react and age to obtain rosin block polyether ;

[0038] 3) Synthesis of comb-type multi-hydrophilic chain rosin block polyether sulfonate: Disperse the rosin block polyether with a solvent, and then pass it through the falling film sulfonation device from the top to flow down along the inner wall, while passing from the top Into SO 3 The mixed gas is fully reacted, aged, removed the solvent, and adjusted the pH value to obtain a comb-shaped polyether sulfonate with multiple hydrophilic chain rosin blocks.

[0039] Preferably, the molar ratio ...

Embodiment 1

[0052] A comb-shaped multi-hydrophilic chain rosin block polyether sulfonate, and its preparation method is as follows:

[0053] 1) Synthesis of aconitic acid-modified rosin: Add crushed rosin (50g, 0.17mol) into a 250mL three-necked flask, heat to 120~130℃ to melt, and then slowly add aconitic acid (28.8g, 0.17) under stirring. mol), and then react at 180~200℃ for 2h to obtain aconitic acid modified rosin;

[0054] 2) Synthesis of rosin block polyether: Add aconitic acid rosin (70g, 0.15mol) into a 500mL stainless steel reactor, stir and heat to 120℃ to melt, add potassium hydroxide (2.7g, 0.05mol), vacuum 0.5 h Remove trace water and low boiling point substances, and then use N 2 Replace the residual air in the reactor, control the reaction temperature at 155~165℃, pressure 0.3~0.4MPa, continuously and stably add propylene oxide (885g, 15mol, 100eq) dropwise, aging and absorb to negative pressure, and then under 0.3~0.4MPa, Continuously and stably add ethylene oxide (660g, 15mol...

Embodiment 2

[0057] A comb-shaped multi-hydrophilic chain rosin block polyether sulfonate, and its preparation method is as follows:

[0058] 1) Synthesis of aconitic acid-modified rosin: In a 250mL three-necked flask, add crushed rosin (50g, 0.17mol), heat to 120~130℃ to melt, then slowly add aconitic acid (57.6g, 0.34mol), then react at 180~200℃ for 3h to obtain aconitic acid modified rosin;

[0059] 2) Synthesis of rosin block polyether: add aconitic acid rosin (70g, 0.15mol) into a 500mL stainless steel reactor, stir and heat to 120℃ to melt, add potassium hydroxide (0.6g, 0.01mol) catalyst, and vacuum 0.5h to remove trace water and low boiling point substances, then use N 2 Replace the residual air in the reactor, control the reaction temperature at 155~165℃, pressure 0.3~0.4MPa, continuously and stably add propylene oxide (708g, 12mol, 80eq) dropwise, aging and absorb to negative pressure, and then under 0.3~0.4MPa, Continuously and stably add ethylene oxide (1056g, 24mol, 160eq), aging ...

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Abstract

The invention discloses a comb-shaped multi-hydrophilic chain rosin block polyether sulfonate and a preparation method thereof. The general structural formula of the rosin block polyether sulfonate is: wherein, m is an integer of 0-100, n is an integer of 0-100, and m and n are not 0 at the same time. The preparation method is as follows: first modify the rosin with aconitic acid to obtain the aconitic acid modified rosin, then polymerize the aconitic acid modified rosin, propylene oxide and ethylene oxide to obtain the rosin block polyether, then SO 3 The rosin block polyether is sulfonated by a falling film method as a sulfonating agent to obtain a comb-shaped multi-hydrophilic chain rosin block polyether sulfonate. The rosin block polyether sulfonate of the present invention has a comb structure, has 4 hydrophilic chains, has strong emulsifying performance, good dispersion stability, and its preparation method is simple, and can be widely used in the emulsification and dispersion of pesticides, coatings, Ink and other fields.

Description

Technical field [0001] The invention relates to a comb-shaped multi-hydrophilic chain rosin block polyether sulfonate and a preparation method thereof, and belongs to the technical field of green surfactants. Background technique [0002] Rosin is widely distributed in Guangdong, Guangxi, Yunnan and other places in my country. It is a renewable resource. Products using rosin as raw materials have been widely used in coatings, pesticides, rubber, medicine, ink, food, electronics and other fields. Rosin has the advantages of being renewable, biodegradable, rich in source, and easy to modify in structure. It is one of the important raw material sources of green surfactants. In 1921, the United States JADecew tried to use rosin sodium salt as a paper sizing agent, marking the beginning of the research and application of surfactants using rosin as raw materials. Subsequently, Germany, Japan, and the former Soviet Union also carried out related research in this regard. Research and us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/326C08G65/26B01F17/44B01F17/52B01F17/02C09K23/02C09K23/44C09K23/52
CPCC08G65/2615C08G65/326C09K23/00
Inventor 贾康乐张雄张磊戴永强苏瑜熊文杰余龙飞高敏文武麦裕良廖兵
Owner INST OF CHEM ENG GUANGDONG ACAD OF SCI
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