Preparation method for polycarboxylic acid series comb-shaped surface active agent

A surfactant and polycarboxylic acid technology, applied in chemical instruments and methods, transportation and packaging, dissolution, etc., can solve problems that are not conducive to marketization, industrialization and environmental protection, consume large solvents and energy, and prolong production cycles. , to achieve the effects of shortening the preparation time, reducing the preparation cost and saving energy

Inactive Publication Date: 2011-09-28
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the end of the polymerization reaction, it is usually necessary to consume a large amount of precipitant to precipitate the main chain polymer and undergo a series of purification steps before it can be used in the next reaction

Method used

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  • Preparation method for polycarboxylic acid series comb-shaped surface active agent

Examples

Experimental program
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Example Embodiment

[0032] Example 1:

[0033] Preparation of poly(methyl methacrylate-co-vinyl acetate)-g-(polyethylene glycol monomethyl ether): Weigh 15.0g methyl methacrylate, 8.6g vinyl acetate, 0.118g azobis Isobutyronitrile, weigh 70mL N,N-dimethylformamide, put each raw material into the reaction kettle at one time, heat and pass nitrogen to make it react at 100°C for 6h. After the reaction is completed, weigh 56.9g polyethylene glycol monomethyl ether (molecular weight 2000), 1.610g sodium ethoxide, measure 30mL N,N-dimethylformamide, and directly add it to the reaction kettle to keep it at 100℃ Reaction 4h. After the reaction was completed, 60% of the solvent in the reaction system was removed under reduced pressure, and then the product was precipitated with cold n-heptane. After filtration under reduced pressure, the filter cake was dissolved with N,N-dimethylformamide, and the dissolved solution was replaced with cold n-heptane. Perform reprecipitation, repeat the dissolution and repr...

Example Embodiment

[0034] Example 2:

[0035] Preparation of poly(vinyl acetate-co-maleic anhydride)-g-(n-butanol): Weigh 12.9g vinyl acetate, 9.8g maleic anhydride, 0.908g azobis-isoheptaonitrile, 0.114g Alkyl mercaptan, weigh 52 mL of N,N-dimethylformamide, put each raw material into the reaction kettle at one time, heat and pass nitrogen to make it react at 100°C for 8 hours. After the reaction is complete, weigh 5.6 g of n-butanol, 2.264 g of p-toluenesulfonic acid, measure 58 mL of N,N-dimethylformamide, and directly add them to the reaction kettle to react at 100°C for 12 hours. After the reaction, 60% of the solvent in the reaction system was removed under reduced pressure, and then the product was precipitated with cold ether. After filtration under reduced pressure, the filter cake was dissolved with N,N-dimethylformamide, and the dissolved solution was re-precipitated with cold ether. The dissolution and reprecipitation were repeated 4 times, and finally the product was dried under reduc...

Example Embodiment

[0036] Example 3:

[0037] Preparation of poly(maleic anhydride-co-acrylic acid)-g-(polyethylene glycol monomethyl ether + n-butanol): Weigh 19.6g maleic anhydride, 7.2g acrylic acid, 1.340g dibenzoyl peroxide, 1.072 g of dodecyl mercaptan, weigh 219 mL of dimethyl sulfoxide, put each raw material into the reaction kettle at one time, and heat and pass nitrogen to make it react at 120°C for 6 hours. After the reaction is complete, weigh 24.3g polyethylene glycol monomethyl ether (molecular weight 550), 5.6g n-butanol, 0.567g p-toluenesulfonic acid, measure 21mL dimethyl sulfoxide, and directly add it to the reactor to make it React at 120°C for 4h. After the reaction is completed, 80% of the solvent in the reaction system is removed under reduced pressure, and then the product is precipitated with cold n-hexane. After filtration under reduced pressure, the filter cake is dissolved with dimethyl sulfoxide, and the dissolved solution is re-precipitated with cold n-hexane. Repeat ...

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Abstract

The invention discloses a preparation method for a polycarboxylic acid series comb-shaped surface active agent, which comprises the following steps of: mixing two comonomers, an initiator, a chain transfer agent and a solvent under the protection of nitrogen, heating to a reacting temperature for polymerization to obtain an intermediate polymer; adding a graft compound, a catalytic agent and a dissolvant into the intermediate polymer, carrying out graft reaction at graft temperature, decompressing and removing part of solvent in a reaction system after reaction, and then precipitating the product with a precipitator; dissolving filter cakes with the solvent; precipitating the dissolved solution with the precipitator again, dissolving repeatedly, precipitating again and then refining, and finally decompressing and drying the product to the constant weight. The preparation method has the advantages of reasonable technology, simple operation, low preparation cost, mild reacting conditions and good product quality.

Description

technical field [0001] The invention belongs to a preparation method of a polymer surfactant, in particular to a preparation method of a polycarboxylic acid series comb-type surfactant. Background technique [0002] Comb-type surfactant is a kind of grafted surfactant. It is composed of several branch chains with different numbers and different molecular structures on a main chain. Its composition is similar to combs in daily life. The shank represents the main chain, and the series of comb teeth represent the side chains. Here, the length, rigidity and flexibility of the main chain can be changed by adjusting the polymerization degree and type of the monomer; the type, length and density of the side chain can also be changed. Due to the regularity, diversity and adjustability of its structure, it has high application value in many fields, especially the polycarboxylate series of comb-type surfactants, because it has a wide range of uses in various industrial fields, so its...

Claims

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Application Information

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IPC IPC(8): C08G81/02C08F220/14C08F218/08C08F222/06C08F220/06C08F212/08C08F228/02B01F17/42C09K23/42
Inventor 杜志平林圣森王万绪王丰收张威台秀梅
Owner CHINA RES INST OF DAILY CHEM IND
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