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Non-ionic anion polysiloxane surfactant and preparation method thereof

A technology of surfactant and polysiloxane, which is applied in the fields of fine chemical industry and material science, can solve the problems of poor product solubility, complex synthesis, and application limitations, and achieve the effects of low production cost, high surface activity, and high yield

Inactive Publication Date: 2009-07-01
汉高股份两合公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] J.Smid et al. have synthesized an anion-containing organosilicon polymer by means of hydrosilylation and epoxy group ring opening, but due to the limitation of the synthesis method, the solubility of the product in water is very poor, and its application is greatly restricted. Limitation of (Polym.Commun, 1989, 30, 52; Macromolecules, 1993, 26, 2202)
[0009] Anionic nonionic polyorganosiloxane as a surfactant has attracted much attention due to its good performance and wide application, but its application is limited due to its complicated synthesis and low yield.

Method used

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  • Non-ionic anion polysiloxane surfactant and preparation method thereof
  • Non-ionic anion polysiloxane surfactant and preparation method thereof
  • Non-ionic anion polysiloxane surfactant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Add 8.7g PDMHS (chemically pure, Hwt% = 0.23, Mn = 1100) (Si-H: 0.02mol) and 6.6g of allyl-terminated polyether (0.01mol, Mn = 660, which shows In the general formula: m=12, n=0, and R is OCCH 3 ), stirring and mixing evenly, the temperature was raised to 90° C., and after nitrogen flow for 10 minutes, adding 0.08ml concentration was 2wt% [Pt] catalyst (isopropanol solution of chloroplatinic acid hexahydrate), after constant temperature reaction for 5 hours, adding 1.37 g of AGE (0.013mol, analytically pure), after continuing the constant temperature reaction for 5 hours, the solvent and excess AGE were evaporated under reduced pressure to obtain 16.3 g of epoxy-containing polyether-polysiloxane with a yield of 99.0 wt%.

[0052] Dissolve the product obtained in the previous step in 75ml of methanol / water mixed solution, raise the temperature to 60°C, add 2.6g of NaHSO 3 (0.025mol, analytically pure), after 48 hours of constant temperature reaction, methanol and most o...

Embodiment 2

[0055] 8g of PDMHS (chemically pure, Hwt% = 0.25, Mn = 1900) (Si-H: 0.02mol) and 8.4g of allyl-terminated polyether (0.012mol, Mn = 700, in its schematic general formula: m=15, n=0, and R is CH 3 ) stirring and mixing evenly, the temperature was raised to 80° C., and after nitrogen flow for 10 minutes, adding 0.08ml concentration was 2wt% [Pt] catalyst (isopropanol solution of chloroplatinic acid hexahydrate), after constant temperature reaction for 6 hours, added 1.42g GMA (0.01 mol, analytically pure), after continuing the constant temperature reaction for 6.5 hours, the excess GMA was evaporated under reduced pressure to obtain 17.3 g of epoxy-containing polyether-polysiloxane with a yield of 98.3 wt%.

[0056] Dissolve the product obtained in the previous step in 75ml of methanol / water mixed solution, raise the temperature to 55°C, add 2.4g of KHSO 3 (0.02mol, analytically pure), after 54 hours of constant temperature reaction, methanol and most of the water were evaporat...

Embodiment 3

[0059] Add 5g PDMHS (chemically pure, Hwt%=0.33, Mn=3000) (Si-H: 0.0165mol) and 9.96g of allyl-terminated polyether (0.0083mol, Mn=1200, which schematically In the general formula: m=20, n=4, and R is H), stir and mix uniformly, be warming up to 100 DEG C, after logical nitrogen 10 minutes, add 0.06ml concentration and be the [Pt] catalyst of 2wt% (chloroplatinum hexahydrate acid 1,1,2,2-tetramethyl-1,2-divinyldisiloxane solution), after constant temperature reaction for 4.5 hours, add 1.14g of AGE (0.01mol, analytically pure), continue constant temperature reaction After 4.5 hours, the solvent and excess AGE were distilled off under reduced pressure to obtain 15.7 g of epoxy group-containing polyether-polysiloxane with a yield of 98.7 wt%.

[0060] Dissolve the product obtained in the previous step in 50ml of methanol / water mixed solution, raise the temperature to 55°C, add 2.28g of Na 2 S 2 o 5 (0.012mol, analytically pure), after 54 hours of constant temperature reaction...

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Abstract

The invention discloses a nonionic-anionic polysiloxane surfactant and a preparation method thereof. The method comprises the following steps: using hydrogen-containing polysiloxane, unsaturated polyether and epoxy-containing unsaturated compounds as raw materials to synthesize epoxy-containing polyether-polysiloxane by adopting two steps of silicon-hydrogen addition reaction, and then making the epoxy-containing polyether-polysiloxane reacted with excessive sulfonating reagent in polar organic solvent / water mixed solvent to prepare the nonionic-anionic polysiloxane surfactant. The preparation has the advantages of easily obtained raw materials for the surfactant, little equipment investment, simple synthesis technology, low production cost and high yield. The molecular weight and the hydrophilic and oleophilic values of the surfactant are controllable; and the surfactant is widely applied in the fields such as textile, papermaking, petrochemical industry, cosmetics, water treatment, environmental improvement, material surface modification and the like, and particularly has good effect on emulsification of special substances in the field of surfactant.

Description

technical field [0001] The invention belongs to the fields of fine chemical industry and material science, more specifically, the invention relates to a nonionic anionic polysiloxane surfactant and a preparation method thereof. Background technique [0002] Polysiloxane surfactant is a new type of surfactant. In addition to excellent wettability, defoaming and low foaming properties, it also has excellent properties such as temperature resistance, weather resistance, non-toxic, non-corrosive and physiological inertness. Therefore, it has a wide range of applications in the fields of textiles, papermaking, petrochemicals, cosmetics, water treatment, environmental governance, and material surface modification. [0003] The research on cationic and nonionic polysiloxane surfactants started earlier, and their preparation methods are more mature, and there are many related application reports and patents. As early as 1967, Dow Corning of the United States applied for the organic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/54C09K23/54
Inventor 阚成友侯昭升赵志清李泽平张勇T·F·利姆
Owner 汉高股份两合公司
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