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Preparation method of isotridecanol polyoxyethylene ether sulfate

A technology of polyoxyethylene ether and isotridecanol, which is applied in the preparation of sulfuric acid amide, chemical instruments and methods, organic chemistry, etc., can solve the problems of time-consuming and energy-consuming, complicated process, and many side reactions, and reduce side reactions. , the effect of simple operation and low production cost

Inactive Publication Date: 2011-07-20
ZHEJIANG HECHENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The two-step method to produce isomeric alcohol ethers is not only complicated, but also time-consuming and energy-consuming, with many side reactions

Method used

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  • Preparation method of isotridecanol polyoxyethylene ether sulfate
  • Preparation method of isotridecanol polyoxyethylene ether sulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Polymerization: Add 275.0 g of isotridecyl alcohol and 2.3 g of sodium methoxide into a 2.5 L pressure reactor, and connect the ethylene oxide metering tank to the pressure reactor. Replace the air with nitrogen for 3 times, wait until the temperature of the kettle rises to 120-125°C, keep the system pressure at 0.2-0.3 MPa, start to feed 181.5g of ethylene oxide, complete the passage in 1.0 hour, and continue the reaction for 1.0 hour. After the reaction is complete, cool down, release the pressure, and filter to remove the filtrate. 456.5 g (1.38 mol) of a reaction product mainly composed of isotridecanol polyoxyethylene ether was obtained, and the molar ratio of isotridecanol to ethylene oxide in the above reaction was 1:3.

[0025] Sulfation reaction: transfer the reaction product obtained from the polymerization reaction to a 1000mL four-neck flask, raise the temperature to 45-50°C, add 41.3g of urea, keep it warm for 0.5 hours, raise the temperature to 75-80°C, ad...

Embodiment 2

[0027] Polymerization reaction: 175.0 g of isotridecyl alcohol and 4.4 g of KOH were added to a 2.5 L pressure reactor, and the ethylene oxide metering tank was connected to the pressure reactor. Replace the air with nitrogen for 3 times, wait until the temperature of the kettle rises to 155-160°C, keep the system pressure at 0.2-0.3MPa, start to feed 269.5g of ethylene oxide, complete the passage in 3 hours, and continue the reaction for 3 hours. After completion of the reaction, cool down, decompress, filter and remove the filter matter, and obtain 444.5 grams (0.88mol) of the reaction product taking isotridecyl alcohol polyoxyethylene ether as the main component. The molar ratio is 1:7.

[0028] Sulfation reaction: transfer the reaction product obtained from the polymerization reaction to a 1000mL four-neck flask, raise the temperature to 55-60°C, add 42.0g of urea, keep it warm for 0.5 hours, raise the temperature to 85-90°C, add 127.3g of sulfamic acid Acid, keep warm fo...

Embodiment 3

[0030] Polymerization reaction: 335.0 g of isotridecyl alcohol and 0.7 g of NaOH were added to a 2.5 L pressure reactor, and the ethylene oxide metering tank was connected to the pressure reactor. Replace the air with nitrogen for 3 times, wait until the temperature of the kettle rises to 80-85°C, keep the system pressure at 0.2-0.3MPa, start feeding 368.5g of ethylene oxide, complete the passage in 1.5 hours, and continue the reaction for 1.5 hours. After completion of the reaction, cool down, decompress, filter and remove the filter matter, and obtain 703.5 grams (1.68mol) of isotridecanyl polyoxyethylene ether as the reaction product of the main component. The molar ratio is 1:5.

[0031] Sulfation reaction: transfer the reaction product obtained from the polymerization reaction to a 1000mL four-necked flask, raise the temperature to 60-65°C, add 20.1g of urea, keep it warm for 0.5 hours, raise the temperature to 90-95°C, add 195.0g of sulfamic acid Acid, keep warm for 2.0...

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Abstract

The invention discloses a preparation method of isotridecanol polyoxyethylene ether sulfate. The method comprises the following steps of: adding epoxy ethane into isotridecanol serving as an initiator in the presence of a basic catalyst by adopting a one-step method and undergoing a polymerization reaction to obtain isotridecanol polyoxyethylene ether; and undergoing a sulfating reaction on the isotridecanol polyoxyethylene ether and sulfamic acid in a programmed temperature raising manner under the catalytic action of urea, and adding a NaOH aqueous solution until the pH value of a reactant is 5-8 to obtain isotridecanol polyoxyethylene sulfate, wherein the molar ratio of the isotridecanol to the epoxy ethane is 1:(3-7), the molar ratio of the isotridecanol polyoxyethylene ether to the sulfamic acid is 1:(0.9-1.5) and the molar ratio of the isotridecanol polyoxyethylene ether to the urea is 1:(0.2-0.8). The preparation method has the characteristics of reduced energy consumption, light product color, good product quality, no three wastes, easiness of operation, small equipment investment and the like.

Description

technical field [0001] The invention relates to a preparation method of isotridecanyl polyoxyethylene ether sulfate, which belongs to the technical field of synthesis of anionic surfactants in organic chemistry. Background technique [0002] The textile pretreatment process is the basic process in the dyeing and finishing production process, and plays an important role in stably improving the product quality of the subsequent processes (dyeing, printing, finishing) and meeting various requirements of customers. The pretreatment process for the dyeing and finishing industry, especially for pure cotton fabrics, the purpose of which is to remove natural impurities on the fabric and additional size additives and contaminants in the weaving process, including the removal of various oils on chemical fiber fabrics And additives, so that the fabric has good wettability, uniform whiteness, better clean appearance, gloss, hand feeling, stable size and strength. In recent years, the e...

Claims

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Application Information

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IPC IPC(8): C07C307/02C07C303/34B01F17/02B01F17/22B01F17/42D06M13/402C09K23/02C09K23/22C09K23/42
Inventor 王伟松金一丰曾红舟王新荣王胜利
Owner ZHEJIANG HECHENG CHEM
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