Preparation method of sulfobetaine type waterborne polyurethane chain extender

A sulfobetaine type, water-based polyurethane technology, applied in the preparation of sulfonic acid, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of difficult reuse, difficult temperature control, low product yield, etc. The production cycle is time-consuming, not easy to agglomerate, and the effect of reducing production costs

Pending Publication Date: 2021-07-20
吉和昌新材料(荆门)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method takes a long time. When the one-pot method is used for synthesis, the temperature is difficult to control, and safety problems are prone to occur in the actual production process. Or when the method of extraction is used for purification, the amount of solvent used is very large, the yield of the final product is low, and different solvents are used in the process of product purification, and it is difficult to process after solvent mixing, and it is difficult to reuse

Method used

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  • Preparation method of sulfobetaine type waterborne polyurethane chain extender
  • Preparation method of sulfobetaine type waterborne polyurethane chain extender

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of N, the preparation method of N-bis(2-hydroxyethyl)-N-methyl-3-sulfonate-1-propylamine, its steps are as follows:

[0030] (1) Add 107.4g of N-methyldiethanolamine into a 1000ml four-necked flask equipped with a thermometer and tetrafluoro stirring, add 280g of anhydrous methanol and stir to dissolve. After complete dissolution, 1 g of powdered potassium hydroxide solid was added. 100g of 1,3-propane sultone is added dropwise under the condition of temperature control at 30-50°C, the dropping time is 1-3h, and the aging time is 1-2h. Two consecutive samples were taken, and the tertiary amine content of the central control sample was calculated to be 2.83% and 2.81% respectively as raw material N-methyldiethanolamine residues. The suspension was cooled to below 20°C, and 247.6g of crude MDAPS was obtained by filtration.

[0031] (2) Use 50ml of methanol to rinse the MDAPS crude product, repeat 2 to 3 times, detect that the sample is basically free of tertiary a...

Embodiment 2

[0033] A kind of N, the preparation method of N-bis(2-hydroxyethyl)-N-methyl-3-sulfonate-1-propylamine, its steps are as follows:

[0034] (1) 102.4g of N-methyldiethanolamine was added to a 1000ml four-neck flask equipped with a thermometer and PTFE stirring, and 280g of methanol recovered in Example 1 was added and stirred to dissolve. After complete dissolution, 1 g of powdered potassium hydroxide solid was added. 100g of 1,3-propane sultone is added dropwise under the condition of temperature control at 30-50°C, the dropping time is 1-3h, and the aging time is 1-2h. Sampling was taken twice in a row, and the tertiary amine content of the central control sample was calculated to be 3.51% and 3.49% respectively as raw material N-methyldiethanolamine residues. The suspension was cooled to below 20°C, and 253.1 g of crude MDAPS was obtained by filtration.

[0035] (2) Rinse the crude MDAPS with 50ml of fresh methanol, repeat 2 to 3 times, detect that the sample is basically f...

Embodiment 3

[0037] A kind of N, the preparation method of N-bis(2-hydroxyethyl)-N-methyl-3-sulfonate-1-propylamine, its steps are as follows:

[0038] (1) Add 356.2g of N-methyldiethanolamine into a 3000ml four-neck flask equipped with a thermometer and PTFE stirring, add 800g of cyclohexane and stir to dissolve. After complete dispersion and dissolution, 5.3 g of potassium methoxide was added. 304.3g of 1,3-propane sultone was added dropwise under the condition of temperature control at 30-50°C, the dropping time was 1-3h, and the aging time was 1-2h. Sampling was taken twice in a row, and the tertiary amine content of the central control sample was calculated to be 4.70% and 4.68% respectively as raw material N-methyldiethanolamine residues. The suspension was cooled to below 20°C, and 732.7g of crude MDAPS was obtained by filtration.

[0039] (2) Use 160ml of fresh cyclohexane to wash the crude MDAPS, repeat 2 to 3 times, detect that the sample has basically no tertiary amine content,...

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Abstract

The invention discloses a preparation method of a sulfobetaine type waterborne polyurethane chain extender, which comprises the following steps: (1) dissolving N-methyldiethanolamine in a solvent, adding a catalyst, uniformly stirring the solution, dropwise adding 1,3-propane sultone, controlling the reaction temperature to be 30-50 DEG C, controlling the dropwise adding time to be 1-3 hours, controlling the aging time to be 1-2 hours, and separating out a product in the reaction process, and then monitoring the mixed turbid liquid through central control sampling, and filtering the liquid to obtain a crude product after the content of tertiary amine is not changed; and (2) spraying and washing the crude product in filtering equipment by using a newly prepared solvent which is the same as that in the step (1) until no tertiary amine content is monitored by central control sampling, filtering, and drying under reduced pressure to obtain the high-purity N,N-bis(2-ethoxyl)-N-methyl-3-sulfonate-1-propylamine. When the emulsion is used for synthesizing the waterborne polyurethane, the emulsification process is convenient to control, the emulsion stability is good, the related mechanical properties and water resistance of the emulsion after a glue film is formed can be improved, and the waterborne polyurethane with high solid content can be synthesized.

Description

technical field [0001] The invention belongs to the technical field of organic compound synthesis, and in particular relates to a preparation method of a sulfobetaine type waterborne polyurethane chain extender. [0002] technical background [0003] Water-based polyurethane can use water as a dispersion medium, abandoning the traditional method of using volatile solvents, and has the characteristics of less pollution, non-toxic and harmless, and there is no big difference in application performance. Mainly used in coatings, leather, coatings and adhesives and other fields. Hydrophilic chain extenders play a key role in water-based polyurethane. Currently, the most commonly used types are carboxylic acid type and sulfonic acid type. [0004] N,N-bis(2-hydroxyethyl)-N-methyl-3-sulfonate-1-propylamine, referred to as MDAPS, is a double-ended hydroxy sulfobetaine type water-based polyurethane chain extender. After the hydrophilic chain extender is introduced into the polyureth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/14C07C303/02C07C303/44C08G18/75C08G18/66C08G18/48C08G18/38
CPCC07C303/02C07C303/44C08G18/755C08G18/6666C08G18/4825C08G18/3855C07C309/14
Inventor 付远波程玄刘凤亮赵樊任凡
Owner 吉和昌新材料(荆门)有限公司
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