Preparing method of high-temperature levelling agent

A technology of high-temperature leveling agent and catalyst, which is applied in dyeing, textiles and papermaking, etc. It can solve the problems of poor leveling effect and refractory degradation of leveling agent, and achieve good dispersion and leveling, high activity and good dispersibility. Effect

Inactive Publication Date: 2019-12-13

陈桂川

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AI-Extracted Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention: Aiming at the problem that the current leveling agent has poor ...

Abstract

The invention relates to a preparing method of a high-temperature levelling agent, and belongs to the technical field of spinning. According to the preparing method, diisopropanol amine and dimethylolpropionic acid are taken as mixed monomers and react with cyclodextrin and the like, a catalyst is adopted for catalysis, a hyperbranched polyester block cyclodextrin substance is formed, a very largecavity is formed in the formed hyperbranched polyester, and many active hydroxide radicals are formed on the surface of the hyperbranched polyester; then the hyperbranched polyester is mixed with a modifying agent formed by butanedioic anhydride and lysine, under the effect of the modifying agent, the content of carboxyl groups on the surface of the polymer can be increased, and the activity is improved; afterwards, glycerinum, cardanol and the like are mixed, and under the effect of a catalyst A, a cardanol-like glyceryl ether substance is formed; finally, the cardanol-like glyceryl ether substance is mixed with the polymer, dimethylformamide, an auxiliary material, an auxiliary agent and the like, wherein the polymer is utilized for triggering a reaction to form polymer-amphiphilic hyperbranched cardanol polyglycidol, and besides, through the utilization of the auxiliary material and the auxiliary agent, the types of active groups can be increased. By means of the preparing method,the problems that current levelling agents have a poor levelling effect and are hard to degrade are solved.

Application Domain

Dyeing process

Technology Topic

Lysine formationPolymeric surface +13

Examples

Experimental program(4)
Comparison scheme(2)
Effect test(1)

Example Embodiment

[0033] A method for preparing a high-temperature leveling agent, the preparation method includes the following steps:

[0034] (1) Based on parts by weight, take 150-160 parts of mixed solvent, 38-52 parts of mixed monomer, 16-22 parts of pentaerythritol, 8-11 parts of modifier, 5-9 parts of cyclodextrin, 1-3 Part of the catalyst, first put the mixed solvent, mixed monomer, pentaerythritol and cyclodextrin into the reaction kettle, protect it with nitrogen, and preheat it at 60°C for 40 minutes;

[0035] (2) After the preheating is over, add the modifier and catalyst, stir and mix, heat up to 110°C, stir for 8h, cool to room temperature, discharge, collect the discharged material, rotate the discharged material to remove the mixed solvent, Collect the residue, mix the residue and acetone at a mass ratio of 1:3~5, mix and stand for 2h, filter, collect the filter residue, and set aside;

[0036] (3) Put glycerin, catalyst A, cardanol and epichlorohydrin into a container at a mass ratio of 4-9:0.3:2~4:16 and mix well, then add 20-30% sodium hydroxide by mass of glycerin. Stir the reaction for 5 hours, remove the epichlorohydrin by rotary evaporation, and collect the residue A;

[0037] (4) Take 160~190 parts of methanol solution, 70~75 parts of dimethylamide, 40~50 parts of residue A, 20~25 parts of spare filter residue, 16~18 parts of auxiliary materials, 6~ Put 13 parts of auxiliary agent and 2-8 parts of accelerator into the reaction kettle, use nitrogen protection, stir and react for 10h at 110~120℃, discharge, collect the discharge mixture, and mix the discharge mixture with ether according to the mass ratio of 1 : 3 mix, stand for 3 hours, centrifuge, collect the centrifuged solids, mix the centrifuged solids and the surfactant at a mass ratio of 7-9:1 to obtain a high-temperature leveling agent.

Example Embodiment

[0038] Example 1

[0039] The mixed solvent is made by mixing xylene and methanol solution in a volume ratio of 7:6.

[0040] The mixed monomer is made by mixing diisopropanolamine and dimethylolpropionic acid in a mass ratio of 1:8.

[0041] The modifier is a mixture of succinic anhydride and lysine at a mass ratio of 11:4.

[0042] The catalyst is a mixture of platinum chloride and p-toluenesulfonic acid in a mass ratio of 7:3.

[0043] Catalyst A is a mixture of benzyltriethylammonium chloride and acetic acid in a mass ratio of 6:5.

[0044] The auxiliary materials are sulfamic acid and urea mixed with a mass ratio of 9:2.

[0045] The auxiliary agent is a mixture of palmitic acid and polyethylene glycol at a mass ratio of 3:6.

[0046] The accelerator is glacial acetic acid.

[0047] The surfactant is alkylphenol polyoxyethylene ether.

[0048] A method for preparing a high-temperature leveling agent, the preparation method includes the following steps:

[0049] (1) In parts by weight, take 160 parts of mixed solvent, 52 parts of mixed monomer, 22 parts of pentaerythritol, 11 parts of modifier, 9 parts of cyclodextrin, and 3 parts of catalyst. Put pentaerythritol and cyclodextrin into the reactor, use nitrogen to protect, preheat at 60℃ for 40min;

[0050] (2) After the preheating is over, add the modifier and catalyst, stir and mix, heat up to 110°C, stir for 8h, cool to room temperature, discharge, collect the discharged material, rotate the discharged material to remove the mixed solvent, Collect the residue, mix the residue and acetone at a mass ratio of 1:5, mix and stand for 2h, filter, and collect the filter residue for use;

[0051] (3) Put glycerin, catalyst A, cardanol and epichlorohydrin into a container at a mass ratio of 9:0.3:4:16 and mix well, then add 30% sodium hydroxide by mass of glycerin, stir and react for 5 hours, and rotatably evaporate Remove epichlorohydrin and collect residue A;

[0052] (4) In parts by weight, take 190 parts of methanol solution, 75 parts of dimethylamide, 50 parts of residue A, 25 parts of spare filter residue, 18 parts of auxiliary materials, 13 parts of auxiliary agents, and 8 parts of accelerators, and put them in In the reactor, using nitrogen protection, stirring at 120°C for 10 hours, discharging, collecting the discharging mixture, mixing the discharging mixture with ether in a mass ratio of 1:3, letting it stand for 3h, centrifuging, and collecting the centrifuged solids. The centrifugal solids and the surfactant are mixed at a mass ratio of 9:1 to obtain a high-temperature levelling agent.

Example Embodiment

[0053] Example 2

[0054] The mixed solvent is made by mixing xylene and methanol solution in a volume ratio of 7:5.

[0055] The mixed monomer is made by mixing diisopropanolamine and dimethylolpropionic acid in a mass ratio of 1:7.

[0056] The modifier is a mixture of succinic anhydride and lysine in a mass ratio of 9:4.

[0057] The catalyst is a mixture of platinum chloride and p-toluenesulfonic acid in a mass ratio of 6:3.

[0058] Catalyst A is a mixture of benzyltriethylammonium chloride and acetic acid in a mass ratio of 6:4.

[0059] The auxiliary materials are sulfamic acid and urea mixed with a mass ratio of 9:1.5.

[0060] The auxiliary agent is a mixture of palmitic acid and polyethylene glycol at a mass ratio of 3:5.

[0061] The accelerator is glacial acetic acid.

[0062] The surfactant is alkylphenol polyoxyethylene ether.

[0063] A method for preparing a high-temperature leveling agent, the preparation method includes the following steps:

[0064] (1) In parts by weight, take 155 parts of mixed solvent, 43 parts of mixed monomer, 20 parts of pentaerythritol, 9 parts of modifier, 8 parts of cyclodextrin, and 2 parts of catalyst. First, mix the mixed solvent, mixed monomer, Put pentaerythritol and cyclodextrin into the reactor, use nitrogen to protect, preheat at 60℃ for 40min;

[0065] (2) After the preheating is over, add the modifier and catalyst, stir and mix, heat up to 110°C, stir for 8h, cool to room temperature, discharge, collect the discharged material, rotate the discharged material to remove the mixed solvent, Collect the residue, mix the residue and acetone at a mass ratio of 1:4, mix and stand for 2 hours, filter, collect the filter residue, and set aside;

[0066] (3) Put glycerin, catalyst A, cardanol and epichlorohydrin into a container at a mass ratio of 6:0.3:3:16 and mix well, then add 25% sodium hydroxide by mass of glycerin, stir and react for 5 hours, and then rotatably evaporate Remove epichlorohydrin and collect residue A;

[0067] (4) In parts by weight, take 180 parts of methanol solution, 73 parts of dimethylamide, 45 parts of residue A, 23 parts of spare filter residue, 17 parts of auxiliary materials, 11 parts of auxiliary agents, and 6 parts of accelerators. In the reactor, use nitrogen protection, stir and react at 115°C for 10 hours, discharge, collect the output mixture, mix the output mixture with ether at a mass ratio of 1:3, stand for 3 hours, centrifuge, and collect the centrifuged solids. The centrifugal solids and the surfactant are mixed at a mass ratio of 8:1 to obtain a high-temperature levelling agent.

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Classification and recommendation of technical efficacy words

Good dispersion
high activity

Preparing method of high-temperature levelling agent

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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