阅读说明：本技术 一种表面活性剂产品及其制备方法和用途 (Surfactant product and preparation method and application thereof ) 是由 张洪飞 盛红艳 吴敏 陆德钟 宋占军 于 2021-08-02 设计创作，主要内容包括：本申请涉及有机化学技术领域,具体公开了一种表面活性剂产品及其制备方法和用途。表面活性剂产品包括通式(Ⅰ)的化合物、通式(Ⅱ)的化合物、通式(Ⅲ)的化合物和通式(Ⅳ)的化合物中的两种或两种以上的混合物；通式(Ⅰ)的化合物、通式(Ⅱ)的化合物、通式(Ⅲ)的化合物和通式(Ⅳ)的化合物的摩尔比为(2-0)：(0-1)：(0-1)：(2-4)。其制备方法是将蓖麻油、环氧丙烷和单异丙醇胺在催化剂作用下依次通过聚合反应和酰胺化反应制得。本申请的制备方法反应条件温和,对设备要求低,且收率高,环境友好,且制得的表面活性剂产品色泽浅、外观透明,配伍性能强,可调控分子量的范围大,表面活性剂产品具有良好的渗透、乳化及分散性能。(The application relates to the technical field of organic chemistry, and particularly discloses a surfactant product, and a preparation method and application thereof. The surfactant product comprises a mixture of two or more of a compound of a general formula (I), a compound of a general formula (II), a compound of a general formula (III) and a compound of a general formula (IV); the molar ratio of the compound of formula (I), the compound of formula (II), the compound of formula (III) and the compound of formula (IV) is (2-0): (0-1): (0-1): (2-4). The preparation method is that the castor oil, the propylene oxide and the monoisopropanolamine are sequentially subjected to polymerization reaction and amidation reaction under the action of a catalyst to obtain the castor oil. The preparation method disclosed by the application has the advantages of mild reaction conditions, low requirements on equipment, high yield and environmental friendliness, and the prepared surfactant product is light in color, transparent in appearance, strong in compatibility, large in range of adjustable molecular weight, and good in permeation, emulsification and dispersion performances.)

1. A surfactant product comprising a mixture of two or more of a compound of formula (i), a compound of formula (ii), a compound of formula (iii) and a compound of formula (iv); the molar ratio of the compound of the general formula (I), the compound of the general formula (II), the compound of the general formula (III) and the compound of the general formula (IV) is (2-0): (0-1): (0-1): (2-4);

wherein R is₁Is- (CH)₂CH₂CH₂O)_n1-H，R₂Is- (CH)₂CH₂CH₂O)_n2-H，R₃Is- (CH)₂CH₂CH₂O)_n3-H，R₄Is- (CH)₂CH₂CH₂O)_n4-H，R₅Is- (CH)₂CH₂CH₂O)_n5-H, n1+ n2+ n5 ═ 3, 4, 5, 6, 7, 8 or 9; n3+ n4+ n5 is 3, 4, 5, 6, 7, 8 or 9.

2. A process for the preparation of a surfactant product according to claim 1, comprising the following steps:

1) reacting castor oil and propylene oxide for 5-15 hours at the temperature of 120-180 ℃ in the presence of an alkaline catalyst;

2) adding monoisopropanolamine into the mixture in the step 1), and reacting for 5-10 hours at the temperature of 100-140 ℃ to obtain a surfactant product;

wherein the molar ratio of castor oil, propylene oxide and monoisopropanolamine is 1: (3-9): (1-2).

3. The method of claim 2, wherein the alkaline catalyst is selected from the group consisting of sodium methoxide, KOH, and NaOH.

4. The method of claim 2, wherein in 1), the degree of reaction is judged by the hydroxyl value: the reaction was stopped when the hydroxyl value ranged from 100-135 mgKOH/g.

5. The method of claim 2, wherein in 2), the reaction degree is judged by the amine value: the reaction was stopped at an amine value in the range of 0.7 to 0.9 mgKOH/g.

6. The method of any one of claims 2-5, wherein when the molar ratio of castor oil to monoisopropanolamine is 1: 1, the surfactant product is composed of a compound of formula (I) and a compound of formula (IV).

7. The method of any one of claims 2-5, wherein when the molar ratio of castor oil to monoisopropanolamine is 1: 2, the surfactant product comprises a compound of a general formula (IV), and the surfactant product also comprises a compound of a general formula (II) and/or a compound of a general formula (III).

8. Use of the surfactant product according to claim 1 for the preparation of a household chemical aid.

Technical Field

The application relates to the technical field of organic chemistry, in particular to a surfactant product, and a preparation method and application thereof.

Background

In the related art, Pluronics series block polyether using propylene glycol as a starting material has good dispersion performance, but the Pluronics series block polyether does not contain a macromolecular lipophilic group, so that the stability of the Pluronics series block polyether in an oil-water mixed solution is poor. Therefore, the development of a new surfactant having an excellent dispersing effect is one of the important issues to be studied in the current daily chemical assistant work.

Disclosure of Invention

In order to improve the dispersion performance of the product, the application provides a surfactant product, and a preparation method and application thereof.

In a first aspect, the present application provides a surfactant product, which adopts the following technical scheme: a surfactant product comprising a mixture of two or more of a compound of formula (i), a compound of formula (ii), a compound of formula (iii) and a compound of formula (iv); the molar ratio of the compound of the general formula (I), the compound of the general formula (II), the compound of the general formula (III) and the compound of the general formula (IV) is (2-0): (0-1): (0-1): (2-4);

wherein R is₁Is- (CH)₂CH₂CH₂O)_n1-H，R₂Is- (CH)₂CH₂CH₂O)_n2-H，R₃Is- (CH)₂CH₂CH₂O)_n3-H，R₄Is- (CH)₂CH₂CH₂O)_n4-H，R₅Is- (CH)₂CH₂CH₂O)_n5-H, n1+ n2+ n5 ═ 3, 4, 5, 6, 7, 8 or 9; n3+ n4+ n5 is 3, 4, 5, 6, 7, 8 or 9.

Preferably, the amine number of the surfactant product is from 0.71 to 0.88 mgKOH/g.

The surfactant product containing multiple active ingredients is obtained by the technical scheme, and the active ingredients are rich in a large number of hydrophilic and lipophilic groups (such as hydroxyl, unsaturated double bonds, ether bonds, ester bonds, amido bonds and the like), so that the hydrophilic and lipophilic groups provide a better dispersing effect for the surfactant product, and the mutual solubility of the components of the surfactant product is improved. Wherein, oxygen atom, nitrogen atom and hydroxyl in ester bond, amido bond and ether bond all have the ability of producing hydrogen bond with water molecule, its stability is high, is difficult to be influenced by strong electrolyte, so has endowed surfactant active product better performance such as dispersion, emulsification and infiltration.

In a second aspect, the present application provides a method for preparing a surfactant product, which adopts the following technical scheme:

a preparation method of a surfactant product comprises the following operation steps:

1) reacting castor oil and propylene oxide for 5-15 hours at the temperature of 120-180 ℃ in the presence of an alkaline catalyst;

2) adding monoisopropanolamine into the mixture in the step 1), and reacting for 5-10 hours at the temperature of 100-140 ℃ to obtain a surfactant product;

wherein the molar ratio of castor oil, propylene oxide and monoisopropanolamine is 1: (3-9): (1-2).

According to the technical scheme, the castor oil, the epoxypropane and the monoisopropanolamine are used as raw materials, and the mixture containing ester bonds, amido bonds, ether bonds, hydroxyl and unsaturated double bonds is prepared through polymerization reaction and amidation reaction in sequence under the action of an alkaline catalyst, wherein nitrogen atoms of the amido bonds, oxygen atoms in the ether bonds and oxygen atoms in the ester bonds and hydroxyl can form hydrogen bonds with water molecules and can interact with the water molecules to form the hydrogen bonds among molecules.

Preferably, the alkaline catalyst is selected from one or more of sodium methoxide, KOH and NaOH.

Preferably, the basic catalyst is added in an amount of 0.1-0.4% by weight based on the weight of castor oil, propylene oxide and monoisopropanolamine.

Preferably, the basic catalyst is added in an amount of 0.2-0.25% by weight based on the weight of castor oil, propylene oxide and monoisopropanolamine.

By adopting the technical scheme, the polymerization reaction and the amidation reaction are carried out by adopting several alkaline catalysts of sodium methoxide, KOH and NaOH, so that the polymerization reaction and the amidation reaction can be simultaneously promoted to be carried out in the positive reaction direction, and the reaction process is accelerated.

Preferably, in 1), the degree of reaction is judged by the hydroxyl value: the reaction was stopped when the hydroxyl value ranged from 100-135 mgKOH/g.

Preferably, in 1), the degree of reaction is judged by the hydroxyl value: the reaction was stopped at a hydroxyl value in the range of 101.8 to 132.9 mgKOH/g.

Preferably, in 2), the degree of reaction is judged by the amine value: the reaction was stopped at an amine value in the range of 0.7 to 0.9 mgKOH/g.

Preferably, in 2), the degree of reaction is judged by the amine value: the reaction was stopped at an amine value in the range of 0.71 to 0.88 mgKOH/g.

By adopting the technical scheme, in the two-step reaction process, the reaction degree is judged by judging the hydroxyl value and the amine value, and compared with the method of simply limiting the reaction time, the performance and the effect of the surfactant product generated by the reaction are more stable.

Preferably, when the molar ratio of the castor oil to the monoisopropanolamine is 1: 1, the surfactant product is composed of a compound of formula (I) and a compound of formula (IV).

By adopting the technical scheme, the castor oil and the monoisopropanolamine are mixed according to the molar ratio of 1: 1, the actual composition of the prepared surfactant product can be effectively controlled by controlling the dosage ratio of the raw materials of the reaction.

Preferably, when the molar ratio of the castor oil to the monoisopropanolamine is 1: 2, the surfactant product comprises a compound of a general formula (IV), and the surfactant product also comprises a compound of a general formula (II) and/or a compound of a general formula (III).

By adopting the technical scheme, the castor oil and the monoisopropanolamine are mixed according to the molar ratio of 1: 2, the actual composition of the prepared surfactant product can be effectively controlled by controlling the dosage ratio of the raw materials of the reaction.

In a third aspect, the present application provides the use of a surfactant product for the preparation of a household chemical aid.

Optimized use of a surfactant product for the preparation of an external additive with dispersing, emulsifying and penetrating effects, selected from the group consisting of cement aids, leather aids and metal processing aids.

In summary, the present application has the following beneficial effects:

1. the surfactant product can be used for preparing a daily chemical additive, a cement additive, a leather additive and a metal processing additive, has the advantage of good dispersion performance, and is green, safe and pollution-free in the preparation method.

2. In the application, the compound containing the general formula (IV) is preferably adopted, the component also comprises ester bonds, amido bonds, ether bonds, hydroxyl groups and unsaturated double bonds, wherein nitrogen atoms in the amido bonds, oxygen atoms in the ester bonds and the hydroxyl groups in the ether bonds can form hydrogen bonds with water molecules, a surfactant product formed by the components has good stability in water, and the compound containing the general formula (IV) can form the hydrogen bonds with the hydroxyl groups, the ether bonds or the ester bonds in other components in the surfactant product through interaction, so that the performances of dispersion, emulsification, permeation and the like of the surfactant product are greatly improved.

3. The preparation method disclosed by the application has the advantages of mild reaction conditions, low requirements on equipment, high yield and environmental friendliness, and the prepared surfactant product is light in color, transparent in appearance, strong in compatibility, large in range of adjustable molecular weight, and good in dispersion, emulsification, permeability and other performances.

Drawings

FIG. 1 is an infrared spectrum of castor oil according to the present application;

FIG. 2 is an infrared spectrum of the surfactant product of example 1 of the present application.

Detailed Description

The present application will be described in further detail with reference to the following drawings and examples.

The raw materials used in the examples of the present application are all commercially available products, except for the following specific descriptions.

The castor oil is selected from castor oil (yellow viscous liquid, water solubility less than 0.1g/100ml at20 deg.C, specification CP: 500ml) produced by Nanjing chemical reagent GmbH.

Examples

Example 1: a surfactant product is prepared by the following steps:

preparation of the reaction kettle before implementation: washing 2.5L high pressure reactor with distilled water for 3 times until clean, oven drying the high pressure reactor, and cooling to 50 deg.C.

1) Adding 965g (1mol) of castor oil and 2.43g of powdery sodium methoxide into a high-pressure reaction kettle, heating to 130 ℃, carrying out vacuum dehydration for 1 hour, adding 174g (3mol) of propylene oxide, and reacting for 15 hours at the temperature of 120 ℃ to obtain an intermediate product; wherein the total dosage of the powdered sodium methoxide accounts for 0.2 percent of the total weight, and the total weight refers to the sum of the weight of castor oil, propylene oxide and monoisopropanolamine.

The assay data for the intermediate at this time are: hydroxyl value 132.9mgKOH/g, molecular weight 1139.

2) Adding 75.11g (1mol) of monoisopropanolamine into the intermediate product generated in the step 1), and reacting at the temperature of 100 ℃ for 10 hours to obtain a surfactant product.

The data determined for the surfactant product of example 1 at this time are: the amine value was 0.86 mgKOH/g.

The surfactant product of example 1 prepared by the above method is composed of the compound of formula (i) and the compound of formula (iv) as can be seen from the infrared data analysis of fig. 1 and 2; and the molar ratio of the compound of the above general formula (I) to the compound of the general formula (IV) is 1: 1.

wherein R is₁Is- (CH)₂CH₂CH₂O)_n1-H，R₂Is- (CH)₂CH₂CH₂O)_n2-H，R₅Is- (CH)₂CH₂CH₂O)_n5-H; n1 is 0, 1, 2 or 3, n2 is 0, 1, 2 or 3, n5 is 0, 1, 2 or 3, and n1+ n2+ n5 is 3.

Example 2: a surfactant product is prepared by the following steps:

preparation of the reaction kettle before implementation: washing a 2.5L high-pressure reaction kettle for 4 times by using distilled water until the reaction kettle is clean, drying the high-pressure reaction kettle, and cooling the high-pressure reaction kettle to 80 ℃ for later use.

1) Adding 965g (1mol) of castor oil and 3.33g of KOH into a high-pressure reaction kettle, heating to 130 ℃, vacuum dehydrating for 1 hour, adding 290g (5mol) of propylene oxide, and reacting for 10 hours at the temperature of 180 ℃ to obtain an intermediate product; wherein, the total KOH consumption accounts for 0.25 percent of the total weight, and the total weight refers to the sum of the weight of castor oil, propylene oxide and monoisopropanolamine.

The assay data for the intermediate at this time are: hydroxyl value 120.6mgKOH/g, molecular weight 1255.

2) Adding 75.11g (1mol) of monoisopropanolamine into the intermediate product generated in the step 1), and reacting at the temperature of 120 ℃ for 8 hours to obtain a surfactant product.

The surfactant product of example 2 now has the following data: the amine value was 0.83 mgKOH/g.

The surfactant product of example 2 obtained by the above preparation method is composed of a compound of the general formula (I) and a compound of the general formula (IV); and the molar ratio of the compound of the above general formula (I) to the compound of the general formula (IV) is 1: 1.

wherein R is₁Is- (CH)₂CH₂CH₂O)_n1-H，R₂Is- (CH)₂CH₂CH₂O)_n2-H，R₅Is- (CH)₂CH₂CH₂O)_n5-H; n1 is 0, 1, 2, 3, 4 or 5, n2 is 0, 1, 2, 3, 4 or 5, n5 is 0, 1, 2, 3, 4 or 5, and n1+ n2+ n5 is 5.

Example 3: a surfactant product is prepared by the following steps:

preparation of the reaction kettle before implementation: washing 2.5L high-pressure reaction kettle with distilled water for 2 times until clean, drying the high-pressure reaction kettle, and cooling to 70 deg.C for use.

1) Adding 965g (1mol) of castor oil and a mixture of 1.25g of KOH and 1.88g of NaOH into a high-pressure reaction kettle, heating to 130 ℃, dehydrating in vacuum for 1 hour, adding 522g (9mol) of propylene oxide, and reacting at 150 ℃ for 8 hours to obtain an intermediate product; wherein, the total dosage of KOH and NaOH is 0.2 percent of the total weight, and the total weight refers to the sum of the weight of castor oil, propylene oxide and monoisopropanolamine.

The assay data for the intermediate at this time are: hydroxyl value of 101.8mgKOH/g, molecular weight of 1487.

2) Adding 75.11g (1mol) of monoisopropanolamine into the intermediate product generated in the step 1), and reacting at the temperature of 140 ℃ for 5 hours to obtain a surfactant product.

The surfactant product of example 3 now has the following data: amine value 0.73 mgKOH/g.

The surfactant product of example 3 obtained by the above preparation method is composed of a compound of the general formula (I) and a compound of the general formula (IV); and the molar ratio of the compound of the above general formula (I) to the compound of the general formula (IV) is 1: 1.

wherein R is₁Is- (CH)₂CH₂CH₂O)_n1-H，R₂Is- (CH)₂CH₂CH₂O)_n2-H，R₅Is- (CH)₂CH₂CH₂O)_n5-H; n1 is 0, 1, 2, 3, 4, 5, 6, 7, 8 or 9, n2 is 0, 1, 2, 3, 4, 5, 6, 7, 8 or 9, n5 is 0, 1, 2, 3, 4, 5, 6, 7, 8 or 9, and n1+ n2+ n5 is 9.

Example 4: a surfactant product is prepared by the following steps:

preparation of the reaction kettle before implementation: washing 2.5L high pressure reactor with distilled water for 3 times until clean, oven drying the high pressure reactor, and cooling to 50 deg.C.

1) Adding 965g (1mol) of castor oil and 2.58g of powdery sodium methoxide into a high-pressure reaction kettle, heating to 130 ℃, carrying out vacuum dehydration for 1 hour, adding 174g (3mol) of propylene oxide, and reacting for 15 hours at the temperature of 120 ℃ to obtain an intermediate product; wherein the total dosage of the powdered sodium methoxide accounts for 0.2 percent of the total weight, and the total weight refers to the sum of the weight of castor oil, propylene oxide and monoisopropanolamine.

The assay data for the intermediate at this time are: hydroxyl value 132.9mgKOH/g, molecular weight 1139.

2) 150.22g (1mol) of monoisopropanolamine is added to the intermediate product generated in the step 1) and the mixture is reacted for 10 hours at the temperature of 100 ℃ to obtain a surfactant product.

The surfactant product of example 4 now has the following data: the amine value was 0.85 mgKOH/g.

The surfactant product of example 4 obtained by the above preparation method is composed of a compound of the general formula (II), a compound of the general formula (III) and a compound of the general formula (IV); and the molar ratio between the sum of the compound of formula (II) and the compound of formula (III) and the compound of formula (IV) is 1: 2.

wherein R is₃Is- (CH)₂CH₂CH₂O)_n3-H，R₄Is- (CH)₂CH₂CH₂O)_n4-H，R₅Is- (CH)₂CH₂CH₂O)_n5-H; n3 is 0, 1, 2 or 3, n4 is 0, 1, 2 or 3, n5 is 0, 1, 2 or 3; and n3+ n4+ n5 is 3.

Example 5: a surfactant product is prepared by the following steps:

preparation of the reaction kettle before implementation: washing a 2.5L high-pressure reaction kettle for 4 times by using distilled water until the reaction kettle is clean, drying the high-pressure reaction kettle, and cooling the high-pressure reaction kettle to 80 ℃ for later use.

1) Adding 965g (1mol) of castor oil and 2.9g of powdery sodium methoxide into a high-pressure reaction kettle, heating to 130 ℃, carrying out vacuum dehydration for 1 hour, adding 348g (6mol) of propylene oxide, and reacting for 15 hours at 120 ℃ to obtain an intermediate product; wherein the total dosage of the powdered sodium methoxide accounts for 0.2 percent of the total weight, and the total weight refers to the sum of the weight of castor oil, propylene oxide and monoisopropanolamine.

The assay data for the intermediate at this time are: hydroxyl value of 115.4mgKOH/g, molecular weight of 1313.

2) 150.22g (1mol) of monoisopropanolamine is added to the intermediate product generated in the step 1) and the mixture is reacted for 10 hours at the temperature of 100 ℃ to obtain a surfactant product.

The surfactant product of example 5 now has the following data: the amine value was 0.81 mgKOH/g.

The surfactant product of example 5 obtained by the above preparation method was composed of the compound of the general formula (II), the compound of the general formula (III) and the compound of the general formula (IV); and the molar ratio between the sum of the compound of formula (II) and the compound of formula (III) and the compound of formula (IV) is 1: 2.

wherein R is₃Is- (CH)₂CH₂CH₂O)_n3-H，R₄Is- (CH)₂CH₂CH₂O)_n4-H，R₅Is- (CH)₂CH₂CH₂O)_n5-H; n3 is 0, 1, 2, 3, 4, 5 or 6, n4 is 0, 1, 2, 3, 4, 5 or 6, n5 is 0, 1, 2, 3, 4, 5 or 6; and n3+ n4+ n5 is 6.

Example 6: a surfactant product is prepared by the following steps:

preparation of the reaction kettle before implementation: washing a 2.5L high-pressure reaction kettle for several times by using distilled water until the reaction kettle is clean, drying the high-pressure reaction kettle, and cooling to 50-80 ℃ for later use.

1) Adding 965g (1mol) of castor oil and 4.1g of KOH into a high-pressure reaction kettle, heating to 130 ℃, carrying out vacuum dehydration for 1 hour, adding 522g (9mol) of propylene oxide, and reacting for 15 hours at the temperature of 120 ℃ to obtain an intermediate product; wherein, the total KOH consumption accounts for 0.25 percent of the total weight, and the total weight refers to the sum of the weight of castor oil, propylene oxide and monoisopropanolamine.

The assay data for the intermediate at this time are: hydroxyl value of 101.8mgKOH/g, molecular weight of 1487.

2) 150.22g (1mol) of monoisopropanolamine is added to the intermediate product generated in the step 1) and the mixture is reacted for 10 hours at the temperature of 100 ℃ to obtain a surfactant product.

The surfactant product of example 6 now has the following data: the amine value was 0.76 mgKOH/g.

The surfactant product of example 6 obtained by the above preparation method was composed of the compound of the general formula (II), the compound of the general formula (III) and the compound of the general formula (IV); and the molar ratio between the sum of the compound of formula (II) and the compound of formula (III) and the compound of formula (IV) is 1: 2.

wherein R is₃Is- (CH)₂CH₂CH₂O)_n3-H，R₄Is- (CH)₂CH₂CH₂O)_n4-H，R₅Is- (CH)₂CH₂CH₂O)_n5-H; n3 is 0, 1, 2, 3, 4, 5, 6, 7, 8 or 9, n4 is 0, 1, 2, 3, 4, 5, 6, 7, 8 or 9, n5 is 0, 1, 2, 3, 4, 5, 6, 7, 8 or 9; and n3+ n4+ n5 is 9.

Performance test

Test one:

test subjects: examples 1 to 6 were used as test samples 1 to 6, and raw material castor oil was used as a control sample 1.

The test method comprises the following steps: the infrared spectra of the test samples 1 to 6 and the control sample 1 were taken, and the infrared data were registered in tables 1 and 2.

TABLE 1 Infrared measurement of Castor oil

TABLE 2

By combining the data of examples 1-6, fig. 1, fig. 2, table 1 and table 2, the infrared spectra of the obtained surfactants all have several characteristic peaks of ether bond, methyl group on propylene oxide and amido bond, thus demonstrating the feasibility of the synthesis process of the present application.

And (2) test II: dispersion, penetration and emulsification Properties test subjects: test subjects: the composite surfactant products prepared in examples 1 to 6 were used as test samples 1 to 6.

The test method comprises the following steps:

1. dispersing ability

1) The experimental basis is as follows: the measurement of the dispersion performance is carried out according to the specification of high-temperature dispersion of the leveling agent for washing the HG/T4261-.

2) The experimental principle is as follows: a leveling agent for washing is added into a disperse dye dyeing working solution, the temperature is raised to 130 ℃, the treatment is carried out for a certain time, then the temperature is lowered to 90 ℃, a vacuum pump is used for suction filtration, the high-temperature dispersibility is evaluated according to the agglomeration condition of residual dye on filter paper, the highest rating result is 5 grades, and the lowest rating result is 1 grade. The high-temperature dispersibility of the leveling agent for washing is characterized by being compared with the stage number of a blank sample without the leveling agent for washing, and the more the stage number is improved, the better the high-temperature dispersibility of the leveling agent for washing is shown.

3) Reagents and materials:

a) dispersing dye: 100% of disperse red jade S-2GFL (C.I. disperse red 167) and 200% of disperse dark blue HGL (C.I. disperse blue 79) can be selected;

b) acetic acid;

c) filter paper: medium speed qualitative filter paper.

4) The experimental steps are as follows:

<1> preparation of dye liquor: the solid content of the polyester resin was measured by the method specified in appendix A, and the following test was performed in terms of the solid content of 20%.

Leveling agent for washing 2.0g/L

Disperse dye 0.5g/L pH value (adjusted by acetic acid) 5.0-5.5

Liquid volume is 100mL

Meanwhile, a blank sample without a leveling agent for washing is prepared for a comparison test.

<2> dye liquor treatment: heating the prepared dye solution to 130 ℃ at the speed of 3.0 ℃/min, preserving the heat for 30min, cooling to 90 ℃ at the speed of 3.0 ℃/min, and preparing for filtration.

<3> filtering the dye liquor: two layers of medium-speed qualitative filter paper are stacked in a Buchner funnel, the filter paper and the Buchner funnel are wetted and preheated by hot water at 90 ℃, a vacuum pump is started, a control valve is adjusted to ensure that the vacuum degree is (0.02 +/-0.005) MPa, and working fluid at 85 ℃ is poured into the Buchner funnel for filtering. And when no liquid drips in the funnel within 10s, turning off the vacuum pump, taking out the filter paper, naturally drying the upper layer of the filter paper, and grading. (attention should be paid to taking the dye liquor and taking protective measures to prevent scalding. attention should be paid to opening the cup to avoid the dye liquor splashing to hurt people due to overlarge pressure) <4> treatment of results

The aggregation of the residual dye particles on the filter paper was assessed and the results were rated as described below, in 9 grades, in that order: 5 stages, 4-5 stages, 4 stages, 3-4 stages, 3 stages, 2-3 stages, 2 stages, 1-2 stages, 1 stage. The worst rating of 1, the best rating of 5, and the average of 3 tests per sample are described in table 3 below, and the average test results are reported in table 4.

The high temperature dispersibility before and after the addition of the leveling agent for washing is compared, and the more the level number is improved after the addition of the leveling agent for washing is carried out, the better the high temperature dispersibility of the leveling agent for washing is shown.

TABLE 3 rating results

2. Permeability capacity

1) The experimental basis is as follows: the solid content was tested according to the specifications of HG/T4266.

2) Principle of experimental evaluation: a shorter settling time indicates better permeability of the sample to the fabric, whereas a longer settling time indicates poorer permeability of the sample to the fabric.

3) Reagents and materials:

a) standard cotton circular canvas sheet: meets the requirements of FZ/T13002 and 2005;

b) the precision of the electronic balance is 0.01 g;

c) a constant-temperature water bath kettle;

d) a stopwatch;

e) a tall flat bottom beaker (. phi.5 cm. times.9.5 cm), 150 mL.

4) The experimental steps are as follows: according to the mass fraction of 25 percent of solid content of a sample, sequentially weighing 1-6 test samples in a clean 150mL high-leg flat-bottom beaker, totaling 6 samples, diluting 1.0g (accurate to 0.01g) of each sample to 100g with water, uniformly stirring, placing in a constant-temperature water bath kettle at 25 ℃ for 0.5h to ensure that the temperature of the solution reaches 25 ℃, horizontally clamping standard canvas, gently placing the canvas on a liquid plane, recording the condition that no foam exists on the liquid surface, pressing a stopwatch while releasing the canvas, and recording the time t1 from wetting to settling to the bottom of the beaker. The test was repeated 5 times, and the average value thereof was recorded as the test result in table 3 in the unit of s.

3. Emulsifying capacity

1) Principle of experiment-phase splitting method

The dispersion of the oil and water phases into an emulsion is a thermodynamically unstable system, and the surfactant has a stabilizing effect on the emulsion. The emulsifying capacity of different surfactants varies. The emulsifying capacity is measured by the time of separation of the oil and water phases of the emulsion, and the longer the time, the more stable the emulsion.

2) Experimental equipment:

a colorimetric tube, a colorimetric tube stand, a stopwatch, a small beaker, a 250mL beaker, a glass rod, a 20mL measuring cylinder, an electronic scale and a ruler.

3) The experimental steps are as follows:

<1>, 100mL of a 0.1% surfactant solution was prepared.

<2>, electronic Scale test samples 1-6 were weighed into 6 small samples each of 10g (i.e., 20 mL). Then 6 small samples are respectively put into a 50mL colorimetric tube with a plug, 10mL of white mineral oil is weighed in a simplified manner and added into the colorimetric tube, the colorimetric tube is shaken vigorously for 10 times after being plugged, the colorimetric tube is stood for one minute and is repeated for five times, the stopwatch is kept still, the stopwatch is immediately pressed until 2.5mL of high water phase is separated, the required time t2(S) is recorded, each surfactant is parallelly done for 2-3 times, and the average value is obtained and recorded in Table 4.

TABLE 4

The data of examples 1-6, commercial products 1-2, and tables 3 and 4 show that the pigments of examples 1-6 all have excellent dispersing ability, all are above grade 4, and the penetration time of examples 1-6 can be controlled within 10 seconds; the emulsifying capacity of the examples 1 to 6 can be controlled within 6h without demixing. It is thus seen that the dispersion, emulsification and penetration properties of examples 1-6 are all greatly enhanced.

And (3) test III:

test subjects: examples 1-6 were used as test samples 1-6, glycerol as a blank, and commercial products 1-2, with 3 swatches per group, for a total of 27 swatches.

The test method comprises the following steps: a total of 9 small samples (5 ml per one small sample), such as test samples 1 to 6, blank samples, and commercial products 1 to 2, were poured into 27 plastic stirring tanks (transparent materials) of 2L together with 1L of glycerin at 25 ℃ under normal pressure, 20ml of methylene blue glycerin solution (i.e., methylene blue-stained glycerin) was added to each plastic stirring tank, and mixed and stirred at 496rpm for 20min using an IKA cantilever stirrer (microsoft 15CONTROL) and an impeller of 3cm in total length, and the average values of the mixing effects of mixing and stirring for 0min, 3min, 10min, and 20min were recorded in table 4. Then, 1L of water was added to 27 plastic stirring barrels of 2L and stirred for 20min, and then the mixture was left standing for 6 hours to observe whether or not there was any delamination, and the observed delamination was recorded in Table 6 below according to the standard for measuring the degree of color difference in Table 5.

TABLE 5 Scoring Scale for color Difference

TABLE 6

Combining the test samples 1-6, the blank samples and the data in tables 5-6, it can be known that, under the stirring speed of 496rpm, the mixing effect of the glycerol solution of methylene blue and glycerol is poor after stirring for 3min, the glycerol solution of methylene blue is not diffused, and at this time, the test samples 1-6 have obvious color difference in the liquid-liquid mixed solution; when the solution is stirred for 10min, a certain color difference still exists at the local part of the liquid-liquid mixed solution; when the stirring time is 20min, the color difference is not obvious, and the uniformity is better. The color difference of the blank sample after being mixed for 10min is close to the mixing effect of the blank sample after being stirred for 3min in the embodiment 1, and the color difference of the blank sample after being mixed for 20min is only half of the color difference of the blank sample after being stirred for 20min in the embodiment 1, so that the dispersing effect of the blank sample after being added into any one of the test samples 1-6 is greatly improved.

Combining the test samples 1-6, the commercial products 1-2, the blank samples and the data in tables 5-6, it can be known that when 1L of water is added and stirred for 20min, standing for 6 hours shows that the test samples 1-6 are integrated with water, no layering phenomenon exists, and the blank samples have obvious layering phenomenon; a small amount of precipitate was also formed at the bottom of the commercial products 1-2, and it was found that examples 1-6 each had good emulsification and delamination prevention effects.

The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.