CN110565412A - Preparation method of high-temperature leveling agent - Google Patents

Preparation method of high-temperature leveling agent Download PDF

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CN110565412A
CN110565412A CN201910704015.9A CN201910704015A CN110565412A CN 110565412 A CN110565412 A CN 110565412A CN 201910704015 A CN201910704015 A CN 201910704015A CN 110565412 A CN110565412 A CN 110565412A
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leveling agent
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陈桂川
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/46General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
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    • D06P1/5264Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
    • D06P1/5271Polyesters; Polycarbonates; Alkyd resins
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    • D06P1/613Polyethers without nitrogen
    • D06P1/6131Addition products of hydroxyl groups-containing compounds with oxiranes
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    • D06P1/62General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds with sulfate, sulfonate, sulfenic or sulfinic groups
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    • D06P1/64General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/642Compounds containing nitrogen
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    • D06P1/653Nitrogen-free carboxylic acids or their salts
    • D06P1/6533Aliphatic, araliphatic or cycloaliphatic

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Abstract

The invention relates to a preparation method of a high-temperature leveling agent, belonging to the technical field of textiles. The invention takes diisopropanolamine and dimethylolpropionic acid as mixed monomers to react with cyclodextrin and the like, hyperbranched polyester block cyclodextrin substances are formed by catalysis of a catalyst, a large cavity is formed in the formed hyperbranched polyester, a plurality of active hydroxyl groups are arranged on the surface, then the hyperbranched polyester block cyclodextrin substances are mixed with a modifier formed by succinic anhydride and lysine, the carboxyl content on the surface of the polymer can be increased by the action of the modifier, the activity is improved, then glycerin, cardanol and the like are mixed, a cardanol-like glyceryl ether substance is formed by the action of the catalyst A, finally the cardanol-like glyceryl ether substance is mixed with the polymer, dimethyl amide, auxiliary materials, auxiliary agents and the like, a polymer-amphiphilic hyperbranched cardanol polyglycidyl glycerol is formed by utilizing the initiation reaction of the polymer, and the problem of poor leveling effect of the existing leveling agent is solved by utilizing the auxiliary materials and the auxiliary materials, and is difficult to degrade.

Description

preparation method of high-temperature leveling agent
Technical Field
The invention relates to a preparation method of a high-temperature leveling agent, belonging to the technical field of textiles.
Background
the polyester fiber is the synthetic fiber with the widest application field and the largest output at present. Because the polyester macromolecular structure of the polyester fiber is compact and the hydrophobicity is strong, the polyester fiber can not be dyed at normal pressure like other fibers, and the polyester fiber is dyed by adopting disperse dye in a high-temperature mode. In addition, in order to save resources and further improve labor productivity, a rapid dyeing method of terylene is mostly adopted, but rapid dyeing is not easy to level, and a leveling agent with excellent dispersibility is required to be added so as to prevent dye from coagulating and have excellent dye transfer performance. The different physical forms of the dyes have great influence on the solubility and the high-temperature dispersion stability of the dyes in water, and directly influence the dyeing properties such as leveling property, dye uptake, lifting property and the like, especially on the terylene superfine fibers.
At present, most high-temperature leveling agents are compounded by anions and nonionic compounds, and the leveling effect is achieved by utilizing the functions of slow dyeing and dye transfer of the nonionic and the dispersing function of the anions. Most of high-temperature leveling agents in the market are aromatic compounds and compounds thereof, can achieve a certain leveling effect, but the leveling effect is not ideal. Therefore, it is necessary to research a high-efficiency high-temperature leveling agent. Patent publication No. 103741519A discloses a high-temperature leveling agent, which is composed of fatty alcohol polyoxyethylene ether, hydroxypropyl methyl cellulose, ethylene glycol fatty acid ester, fatty amine polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, glycerol trioleate and tartaric acid in different proportions. But the level dyeing effect is not good, and the slow dyeing, the transfer dyeing and the dispersion effect are poor.
In addition, a plurality of high-temperature leveling agents such as glyceryl ether oleate is compounded with styryl phenol polyoxyethylene ether sulfate to form GS; a high-temperature leveling agent FZ compounded by fatty alcohol-polyoxyethylene ether and sodium alkyl benzene sulfonate, and the like. The high-temperature leveling agents are all relatively excellent and commonly used products in the market, and have various advantages in effect performance-price ratio. For example, the GS type is one of the types which are widely used in the current market, and the dyeing requirement can be met when the general usage amount is about 0.5 percent. However, although the high-temperature leveling agents have certain effects, and the GS and FZ types have good effects, the high-temperature leveling agents contain styrol and phenol substances, and the styrol and phenol components are difficult to degrade and are not environment-friendly, and belong to international banned products.
disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems of poor leveling effect and difficult degradation of the existing leveling agent, the invention provides a preparation method of a high-temperature leveling agent.
In order to solve the technical problems, the invention adopts the following technical scheme:
A preparation method of a high-temperature leveling agent comprises the following steps:
(1) taking 150-160 parts by weight of mixed solvent, 38-52 parts by weight of mixed monomer, 16-22 parts by weight of pentaerythritol, 8-11 parts by weight of modifier, 5-9 parts by weight of cyclodextrin and 1-3 parts by weight of catalyst, firstly putting the mixed solvent, the mixed monomer, the pentaerythritol and the cyclodextrin into a reaction kettle, and using nitrogen for protection and preheating;
(2) After preheating is finished, adding a modifier and a catalyst, stirring and mixing, heating, stirring for reaction, cooling, discharging, collecting a discharged material, performing rotary evaporation on the discharged material to remove a mixed solvent, collecting a remainder, mixing the remainder and acetone according to a mass ratio of 1: 3-5, standing, filtering, and collecting filter residues for later use;
(3) Putting glycerol, a catalyst A, cardanol and epichlorohydrin into a container according to a mass ratio of 4-9: 0.3: 2-4: 16, uniformly mixing, adding sodium hydroxide with the mass being 20-30% of that of the glycerol, stirring for reaction, performing rotary evaporation to remove the epichlorohydrin, and collecting a residue A;
(4) According to the weight parts, 160-190 parts of methanol solution, 70-75 parts of dimethyl amide, 40-50 parts of residue A, 20-25 parts of standby filter residue, 16-18 parts of auxiliary materials, 6-13 parts of auxiliary agents and 2-8 parts of promoters are put into a reaction kettle, stirred and reacted at 110-120 ℃ under the protection of nitrogen, discharged, a discharged mixture is collected, the discharged mixture and ethyl ether are mixed according to the mass ratio of 1:3, standing and centrifuging are carried out, a centrifuged solid is collected, and the centrifuged solid and a surfactant are mixed according to the mass ratio of 7-9: 1, so that the high-temperature leveling agent is obtained.
the mixed solvent in the step (1) is prepared by mixing dimethylbenzene and a methanol solution according to a volume ratio of 7: 3-6.
The mixed monomer in the step (1) is formed by mixing diisopropanolamine and dimethylolpropionic acid according to the mass ratio of 1: 5-8.
The modifier in the step (1) is formed by mixing succinic anhydride and lysine according to a mass ratio of 8-11: 4.
The catalyst is formed by mixing platinum chloride and p-toluenesulfonic acid according to a mass ratio of 5-7: 3.
The catalyst A in the step (3) is formed by mixing benzyltriethylammonium chloride and acetic acid according to the mass ratio of 6: 3-5.
In the step (4), the auxiliary materials are prepared by mixing sulfamic acid and urea according to the mass ratio of 9: 1-2.
The auxiliary agent in the step (4) is formed by mixing palmitic acid and polyethylene glycol according to the mass ratio of 3: 4-6.
The accelerant in the step (4) is glacial acetic acid.
and (4) the surfactant in the step (4) is alkylphenol polyoxyethylene.
Compared with other methods, the method has the beneficial technical effects that:
(1) The invention takes diisopropanolamine and dimethylolpropionic acid as mixed monomers to react with cyclodextrin and the like, and forms hyperbranched polyester block cyclodextrin substances through the catalysis of a catalyst, the formed hyperbranched polyester has a large cavity inside and a plurality of active hydroxyl groups on the surface, and is mixed with a modifier formed by succinic anhydride and lysine, the carboxyl content of the surface of the polymer can be increased through the action of the modifier, the activity is improved, then glycerin, cardanol and the like are mixed, forming cardanol-like glycerol ether substance under the action of the catalyst A, finally mixing with polymer, dimethyl amide, auxiliary materials, auxiliary agents and the like, by utilizing a polymer to initiate reaction, polymer-amphiphilic hyperbranched cardanol polyglycidyl glycerol is formed, and the types of active groups can be improved by utilizing auxiliary materials and auxiliary materials;
(2) When the invention is used, firstly, the high-activity polymer-amphiphilic hyperbranched cardanol polyglycidyl glycerol can be well dispersed, meanwhile, because the dye contains a large number of active groups such as hydroxyl, amino and the like and has ion repulsion with the groups such as hydroxyl, amino and the like in the dye molecules, can achieve good dispersibility and solubilization effects, but at the same time, the leveling agent of the invention also contains partial phenolic hydroxyl, and can be adsorbed with dye molecules by Van der Waals force, but also can form hydrogen bonds with hydroxyl, amino and the like in dye molecules, and as the bonding strength of the hydrogen bonds is greater than the strength of Van der Waals force, so that the dye is combined with dye particles more firmly at high temperature, and can play a good role in dispersing and leveling, therefore, through two opposite effects in the leveling agent, the leveling agent can play a good leveling and dispersing effect, and meanwhile, the prepared leveling agent has good degradability.
Detailed Description
The mixed solvent is prepared by mixing dimethylbenzene and methanol solution according to the volume ratio of 7: 3-6.
the mixed monomer is formed by mixing diisopropanolamine and dimethylolpropionic acid according to the mass ratio of 1: 5-8.
The modifier is formed by mixing succinic anhydride and lysine according to the mass ratio of 8-11: 4.
The catalyst is formed by mixing platinum chloride and p-toluenesulfonic acid according to a mass ratio of 5-7: 3.
The catalyst A is formed by mixing benzyltriethylammonium chloride and acetic acid according to the mass ratio of 6: 3-5.
The auxiliary material is formed by mixing sulfamic acid and urea according to the mass ratio of 9: 1-2.
The auxiliary agent is formed by mixing palmitic acid and polyethylene glycol according to the mass ratio of 3: 4-6.
The promoter is glacial acetic acid.
The surfactant is alkylphenol polyoxyethylene.
A preparation method of a high-temperature leveling agent comprises the following steps:
(1) Taking 150-160 parts by weight of mixed solvent, 38-52 parts by weight of mixed monomer, 16-22 parts by weight of pentaerythritol, 8-11 parts by weight of modifier, 5-9 parts by weight of cyclodextrin and 1-3 parts by weight of catalyst, firstly putting the mixed solvent, the mixed monomer, the pentaerythritol and the cyclodextrin into a reaction kettle, using nitrogen for protection, and preheating for 40min at 60 ℃;
(2) after preheating is finished, adding a modifier and a catalyst, stirring and mixing, heating to 110 ℃, stirring and reacting for 8 hours, cooling to room temperature, discharging, collecting discharged materials, performing rotary evaporation on the discharged materials to remove a mixed solvent, collecting residues, mixing the residues and acetone according to a mass ratio of 1: 3-5, standing for 2 hours, filtering, and collecting filter residues for later use;
(3) Putting glycerol, a catalyst A, cardanol and epichlorohydrin into a container according to a mass ratio of 4-9: 0.3: 2-4: 16, uniformly mixing, adding sodium hydroxide with the mass being 20-30% of that of the glycerol, stirring for reaction for 5 hours, performing rotary evaporation to remove the epichlorohydrin, and collecting a residue A;
(4) According to the weight parts, 160-190 parts of methanol solution, 70-75 parts of dimethyl amide, 40-50 parts of residue A, 20-25 parts of standby filter residue, 16-18 parts of auxiliary materials, 6-13 parts of auxiliary agents and 2-8 parts of promoters are put into a reaction kettle, stirred and reacted for 10 hours at 110-120 ℃ under the protection of nitrogen, discharged materials are collected, the discharged material mixture is mixed with ethyl ether according to the mass ratio of 1:3, the mixture is kept stand for 3 hours, centrifuged solids are collected, and the centrifuged solids and a surfactant are mixed according to the mass ratio of 7-9: 1 to obtain the high-temperature leveling agent.
Example 1
The mixed solvent is prepared by mixing dimethylbenzene and methanol solution according to the volume ratio of 7: 6.
The mixed monomer is formed by mixing diisopropanolamine and dimethylolpropionic acid according to the mass ratio of 1: 8.
the modifier is formed by mixing succinic anhydride and lysine according to the mass ratio of 11: 4.
The catalyst is formed by mixing platinum chloride and p-toluenesulfonic acid according to the mass ratio of 7: 3.
the catalyst A is prepared by mixing benzyltriethylammonium chloride and acetic acid according to the mass ratio of 6: 5.
The auxiliary material is prepared by mixing sulfamic acid and urea according to the mass ratio of 9: 2.
the auxiliary agent is formed by mixing palmitic acid and polyethylene glycol according to the mass ratio of 3: 6.
The promoter is glacial acetic acid.
The surfactant is alkylphenol polyoxyethylene.
A preparation method of a high-temperature leveling agent comprises the following steps:
(1) Taking 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 according to parts by weight, firstly putting the mixed solvent, the mixed monomer, the pentaerythritol and the cyclodextrin into a reaction kettle, using nitrogen for protection, and preheating for 40min at 60 ℃;
(2) After preheating is finished, adding a modifier and a catalyst, stirring and mixing, heating to 110 ℃, stirring and reacting for 8 hours, cooling to room temperature, discharging, collecting discharged materials, performing rotary evaporation on the discharged materials to remove a mixed solvent, collecting residues, mixing and standing the residues and acetone according to a mass ratio of 1:5 for 2 hours, filtering, and collecting filter residues for later use;
(3) Putting glycerol, a catalyst A, cardanol and epichlorohydrin into a container according to a mass ratio of 9:0.3:4:16, uniformly mixing, adding sodium hydroxide accounting for 30% of the mass of the glycerol, stirring for reaction for 5 hours, carrying out rotary evaporation to remove the epichlorohydrin, and collecting a remainder A;
(4) according to the weight parts, 190 parts of methanol solution, 75 parts of dimethyl amide, 50 parts of remainder A, 25 parts of standby filter residue, 18 parts of auxiliary materials, 13 parts of auxiliary agents and 8 parts of promoters are put into a reaction kettle, stirred and reacted for 10 hours at 120 ℃ under the protection of nitrogen, discharged materials are collected, discharged material mixtures are collected, the discharged material mixtures and ethyl ether are mixed according to the mass ratio of 1:3, the mixture is kept stand for 3 hours, centrifuged solids are collected, and the centrifuged solids and surfactants are mixed according to the mass ratio of 9:1, so that the high-temperature leveling agent is obtained.
Example 2
The mixed solvent is prepared by mixing dimethylbenzene and methanol solution according to the volume ratio of 7: 5.
The mixed monomer is formed by mixing diisopropanolamine and dimethylolpropionic acid according to the mass ratio of 1: 7.
The modifier is formed by mixing succinic anhydride and lysine according to the mass ratio of 9: 4.
The catalyst is formed by mixing platinum chloride and p-toluenesulfonic acid according to the mass ratio of 6: 3.
The catalyst A is prepared by mixing benzyltriethylammonium chloride and acetic acid according to the mass ratio of 6: 4.
The auxiliary material is prepared by mixing sulfamic acid and urea according to the mass ratio of 9: 1.5.
The auxiliary agent is formed by mixing palmitic acid and polyethylene glycol according to the mass ratio of 3: 5.
The promoter is glacial acetic acid.
the surfactant is alkylphenol polyoxyethylene.
A preparation method of a high-temperature leveling agent comprises the following steps:
(1) according to the weight parts, 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 are taken, firstly, the mixed solvent, the mixed monomer, the pentaerythritol and the cyclodextrin are put into a reaction kettle, nitrogen is used for protection, and preheating is carried out for 40min at 60 ℃;
(2) After preheating is finished, adding a modifier and a catalyst, stirring and mixing, heating to 110 ℃, stirring and reacting for 8 hours, cooling to room temperature, discharging, collecting discharged materials, performing rotary evaporation on the discharged materials to remove a mixed solvent, collecting residues, mixing and standing the residues and acetone according to a mass ratio of 1:4 for 2 hours, filtering, and collecting filter residues for later use;
(3) Putting glycerol, a catalyst A, cardanol and epichlorohydrin into a container according to a mass ratio of 6:0.3:3:16, uniformly mixing, adding sodium hydroxide accounting for 25% of the mass of the glycerol, stirring for reaction for 5 hours, carrying out rotary evaporation to remove the epichlorohydrin, and collecting a remainder A;
(4) Taking 180 parts of methanol solution, 73 parts of dimethyl amide, 45 parts of remainder A, 23 parts of standby filter residue, 17 parts of auxiliary materials, 11 parts of auxiliary agents and 6 parts of promoters, putting the mixture into a reaction kettle, stirring and reacting the mixture at 115 ℃ for 10 hours under the protection of nitrogen, discharging, collecting a discharged mixture, mixing the discharged mixture with diethyl ether according to the mass ratio of 1:3, standing the mixture for 3 hours, centrifuging the mixture, collecting a centrifuged solid, and mixing the centrifuged solid with a surfactant according to the mass ratio of 8:1 to obtain the high-temperature leveling agent.
example 3
the mixed solvent is prepared by mixing dimethylbenzene and methanol solution according to the volume ratio of 7: 3.
The mixed monomer is prepared by mixing diisopropanolamine and dimethylolpropionic acid according to the mass ratio of 1: 5.
The modifier is formed by mixing succinic anhydride and lysine according to the mass ratio of 8: 4.
The catalyst is formed by mixing platinum chloride and p-toluenesulfonic acid according to the mass ratio of 5: 3.
The catalyst A is prepared by mixing benzyltriethylammonium chloride and acetic acid according to the mass ratio of 6: 3.
The auxiliary material is prepared by mixing sulfamic acid and urea according to the mass ratio of 9:1.
The auxiliary agent is formed by mixing palmitic acid and polyethylene glycol according to the mass ratio of 3: 4.
The promoter is glacial acetic acid.
the surfactant is alkylphenol polyoxyethylene.
A preparation method of a high-temperature leveling agent comprises the following steps:
(1) Taking 150 parts of mixed solvent, 38 parts of mixed monomer, 16 parts of pentaerythritol, 8 parts of modifier, 5 parts of cyclodextrin and 1 part of catalyst according to parts by weight, firstly putting the mixed solvent, the mixed monomer, the pentaerythritol and the cyclodextrin into a reaction kettle, using nitrogen for protection, and preheating for 40min at 60 ℃;
(2) After preheating is finished, adding a modifier and a catalyst, stirring and mixing, heating to 110 ℃, stirring and reacting for 8 hours, cooling to room temperature, discharging, collecting discharged materials, performing rotary evaporation on the discharged materials to remove a mixed solvent, collecting residues, mixing the residues and acetone according to a mass ratio of 1:3, standing for 2 hours, filtering, and collecting filter residues for later use;
(3) Putting glycerol, a catalyst A, cardanol and epichlorohydrin into a container according to a mass ratio of 4:0.3:2:16, uniformly mixing, adding sodium hydroxide accounting for 20% of the mass of the glycerol, stirring for reaction for 5 hours, carrying out rotary evaporation to remove the epichlorohydrin, and collecting a remainder A;
(4) According to the weight parts, 160 parts of methanol solution, 70 parts of dimethyl amide, 40 parts of remainder A, 20 parts of standby filter residue, 16 parts of auxiliary materials, 6 parts of auxiliary agents and 2 parts of promoters are put into a reaction kettle, stirred and reacted for 10 hours at 110 ℃ under the protection of nitrogen, discharged materials are collected, discharged material mixtures are collected, the discharged material mixtures and ethyl ether are mixed according to the mass ratio of 1:3, the mixture is kept stand for 3 hours, centrifuged solids are collected, and the centrifuged solids and surfactants are mixed according to the mass ratio of 7:1, so that the high-temperature leveling agent is obtained.
Comparative example 1
the mixed solvent is prepared by mixing dimethylbenzene and methanol solution according to the volume ratio of 7: 5.
The mixed monomer is formed by mixing diisopropanolamine and dimethylolpropionic acid according to the mass ratio of 1: 7.
The modifier is formed by mixing succinic anhydride and lysine according to the mass ratio of 9: 4.
The catalyst is formed by mixing platinum chloride and p-toluenesulfonic acid according to the mass ratio of 6: 3.
The catalyst A is prepared by mixing benzyltriethylammonium chloride and acetic acid according to the mass ratio of 6: 4.
the auxiliary material is prepared by mixing sulfamic acid and urea according to the mass ratio of 9: 1.5.
the auxiliary agent is formed by mixing palmitic acid and polyethylene glycol according to the mass ratio of 3: 5.
the promoter is glacial acetic acid.
the surfactant is alkylphenol polyoxyethylene.
A preparation method of a high-temperature leveling agent comprises the following steps:
(1) According to the weight parts, 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 are taken, firstly, the mixed solvent, the mixed monomer, the pentaerythritol and the cyclodextrin are put into a reaction kettle, nitrogen is used for protection, and preheating is carried out for 40min at 60 ℃;
(2) After preheating is finished, adding a modifier and a catalyst, stirring and mixing, heating to 110 ℃, stirring and reacting for 8 hours, cooling to room temperature, discharging, collecting discharged materials, performing rotary evaporation on the discharged materials to remove a mixed solvent, collecting residues, mixing and standing the residues and acetone according to a mass ratio of 1:4 for 2 hours, filtering, and collecting filter residues for later use;
(3) putting glycerol, a catalyst A, cardanol and epichlorohydrin into a container according to a mass ratio of 6:0.3:3:16, uniformly mixing, adding sodium hydroxide accounting for 25% of the mass of the glycerol, stirring for reaction for 5 hours, carrying out rotary evaporation to remove the epichlorohydrin, and collecting a remainder A;
(4) Taking 180 parts of methanol solution, 73 parts of dimethyl amide, 45 parts of remainder A, 23 parts of standby filter residue, 17 parts of auxiliary materials, 11 parts of auxiliary agents and 6 parts of promoters by weight parts, putting the mixture into a reaction kettle, stirring and reacting the mixture at 115 ℃ for 10 hours under the protection of nitrogen, discharging, collecting a discharged mixture, mixing the discharged mixture with diethyl ether according to the mass ratio of 1:3, standing for 3 hours, centrifuging, collecting a centrifuged solid, and obtaining the high-temperature leveling agent.
comparative example 2
A commercially available leveling agent.
And (3) carrying out dye uptake, fixation rate and levelling property tests on the pure cotton fabric obtained by dyeing the levelling agents in the above examples and comparative examples, wherein the dye uptake is as follows: and measuring residual liquid before and after dyeing on a spectrophotometer to obtain the dye uptake of the dye. And (3) fixation rate: and drying the pure cotton fabric before and after dyeing in an oven at 100 ℃ to an absolute dry weight, dyeing and measuring, wherein the fixation rate of the dye on the pure cotton fabric is obtained by dividing the dyed pure cotton fabric by the pure cotton fabric before dyeing. Leveling property: selecting one point on the fabric as a standard point, then randomly selecting 10 points, testing the color difference value, calculating the standard deviation S, wherein the smaller the value of the standard deviation S, the better the leveling property, and detecting whether the leveling agent described in the examples and the comparative examples has difficultly degraded substances such as styrenated phenol, phenol and the like, and the specific results are shown in the following table 1.
Table 1:
Detecting items Example 1 Example 2 example 3 Comparative example 1 comparative example 2
The dye uptake rate% 98.0~99.4 98.3~99.5 97.5~99.3 98.2~99.4 97.3~98.2
Color fixing rate% 95.7~97.0 95.8~97.2 95.5~96.8 98.7~97.1 94.3~96.1
Levelling property 1.32~1.55 1.30~1.5 1.35~1.52 1.31~1.52 1.36~1.59
Whether or not it contains a hardly degradable substance Whether or not whether or not Whether or not Whether or not is that
from the above, it can be seen that the leveling agent of the present invention is better and more suitable for popularization and application in table 1, and the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims (10)

1. The preparation method of the high-temperature leveling agent is characterized by comprising the following steps of:
(1) Taking 150-160 parts by weight of mixed solvent, 38-52 parts by weight of mixed monomer, 16-22 parts by weight of pentaerythritol, 8-11 parts by weight of modifier, 5-9 parts by weight of cyclodextrin and 1-3 parts by weight of catalyst, firstly putting the mixed solvent, the mixed monomer, the pentaerythritol and the cyclodextrin into a reaction kettle, and using nitrogen for protection and preheating;
(2) After preheating is finished, adding a modifier and a catalyst, stirring and mixing, heating, stirring for reaction, cooling, discharging, collecting a discharged material, performing rotary evaporation on the discharged material to remove a mixed solvent, collecting a remainder, mixing the remainder and acetone according to a mass ratio of 1: 3-5, standing, filtering, and collecting filter residues for later use;
(3) putting glycerol, a catalyst A, cardanol and epichlorohydrin into a container according to a mass ratio of 4-9: 0.3: 2-4: 16, uniformly mixing, adding sodium hydroxide with the mass being 20-30% of that of the glycerol, stirring for reaction, performing rotary evaporation to remove the epichlorohydrin, and collecting a residue A;
(4) According to the weight parts, 160-190 parts of methanol solution, 70-75 parts of dimethyl amide, 40-50 parts of residue A, 20-25 parts of standby filter residue, 16-18 parts of auxiliary materials, 6-13 parts of auxiliary agents and 2-8 parts of promoters are put into a reaction kettle, stirred and reacted at 110-120 ℃ under the protection of nitrogen, discharged, a discharged mixture is collected, the discharged mixture and ethyl ether are mixed according to the mass ratio of 1:3, standing and centrifuging are carried out, a centrifuged solid is collected, and the centrifuged solid and a surfactant are mixed according to the mass ratio of 7-9: 1, so that the high-temperature leveling agent is obtained.
2. The preparation method of the high-temperature leveling agent according to claim 1, wherein the mixed solvent in the step (1) is prepared by mixing xylene and methanol solution according to a volume ratio of 7: 3-6.
3. The preparation method of the high-temperature leveling agent according to claim 1, wherein the mixed monomer in the step (1) is prepared by mixing diisopropanolamine and dimethylolpropionic acid according to a mass ratio of 1: 5-8.
4. The preparation method of the high-temperature leveling agent according to claim 1, wherein the modifier in the step (1) is prepared by mixing succinic anhydride and lysine according to a mass ratio of 8-11: 4.
5. The preparation method of the high-temperature leveling agent according to claim 1, wherein the catalyst is formed by mixing platinum chloride and p-toluenesulfonic acid according to a mass ratio of 5-7: 3.
6. The preparation method of the high-temperature leveling agent according to claim 1, wherein the catalyst A in the step (3) is prepared by mixing benzyltriethylammonium chloride and acetic acid according to a mass ratio of 6: 3-5.
7. The preparation method of the high-temperature leveling agent according to claim 1, wherein in the step (4), the auxiliary materials are prepared by mixing sulfamic acid and urea according to a mass ratio of 9: 1-2.
8. The preparation method of the high-temperature leveling agent according to claim 1, wherein the adjuvant in the step (4) is formed by mixing palmitic acid and polyethylene glycol according to a mass ratio of 3: 4-6.
9. the method for preparing a high-temperature leveling agent according to claim 1, wherein the accelerator in the step (4) is glacial acetic acid.
10. the method for preparing the high-temperature leveling agent according to claim 1, wherein the surfactant in the step (4) is alkylphenol ethoxylate.
CN201910704015.9A 2019-08-01 2019-08-01 Preparation method of high-temperature leveling agent Withdrawn CN110565412A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115538194A (en) * 2022-11-10 2022-12-30 苏州联胜化学有限公司 Disperse dyeing anti-flocculation leveling agent and synthetic method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115538194A (en) * 2022-11-10 2022-12-30 苏州联胜化学有限公司 Disperse dyeing anti-flocculation leveling agent and synthetic method thereof
CN115538194B (en) * 2022-11-10 2023-11-03 苏州联胜化学有限公司 Disperse dyeing deflocculating leveling agent and synthesis method thereof

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Application publication date: 20191213