CN114107579B - Preparation method of phosphate fatliquor - Google Patents
Preparation method of phosphate fatliquor Download PDFInfo
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- CN114107579B CN114107579B CN202111481003.8A CN202111481003A CN114107579B CN 114107579 B CN114107579 B CN 114107579B CN 202111481003 A CN202111481003 A CN 202111481003A CN 114107579 B CN114107579 B CN 114107579B
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- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C9/00—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes
- C14C9/02—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes using fatty or oily materials, e.g. fat liquoring
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Abstract
The invention discloses a preparation method of a phosphate fatliquor, which comprises the following steps of firstly preparing an alkylolamide product; then adding C12-14 fatty alcohol and polyisobutylene 950, adding phosphorus pentoxide, performing a phosphorylation reaction at a certain temperature to obtain a product with phosphate monoester, phosphate diester and phosphate triester as main components, and then adding an emulsifier and a certain amount of water for emulsification; then adding 35% sodium hydroxide solution to adjust the pH value; then, 50 percent sodium acetate solution is used for regulating the fluidity, and finally, the novel synthetic phosphate ester-adding agent is prepared. The phosphate fat-liquoring agent is a high-efficiency multifunctional active substance simultaneously containing amino and phosphoryl, can act with carboxyl and amino in leather fibers to form a complex with protein, and plays a good role in fat-liquoring and filling. Meanwhile, the P = O bond in the phosphate functional group has strong complexation with chromium in the leather, so that the synthetic phosphate type fatting agent has long fatting effect on the leather, and the leather is soft, full, elastic and moist in hand feeling.
Description
Technical Field
The invention relates to the field of preparation of a fatting agent, and in particular relates to a preparation method of a phosphate fatting agent.
Background
Leather fatliquoring is one of the important processes in the leather production process, and is to treat leather with fatliquoring agent to make the leather absorb a certain amount of grease so as to endow the leather with certain physical and mechanical properties and service performance. The leather greasing function is to make the leather soft, plump, folding-resistant and elastic; the tensile strength and the waterproofness are improved; can also slightly supplement tanning, filling, dyeing and color fixing and slow down the outward migration of the tanning agent. The leather fatting agent mainly comprises neutral oil and emulsified components, the grease components in the fatting agent are different, and leather treated by greasing in the menstrual period also has different styles; however, the leather fatting agent on the market at present has poor acid resistance, alkali resistance, salt resistance stability and permeability, and single performance, and can not meet the requirements of the leather fatting process.
Disclosure of Invention
The invention aims to provide a preparation method of a phosphate fatliquor, and the phosphate fatliquor prepared by the method has good acid resistance, alkali resistance and salt resistance, can endow leather with the properties of softness, fullness and moist touch, and is used for solving the technical problems in the background technology.
The technical scheme of the invention provides a preparation method of a phosphate fatliquor, which comprises the following steps:
s1: 880-890 parts of alkylolamides, 540-550 parts of C12-14 fatty alcohols and 160-170 parts of polyisobutylene 950 are added into a reactor, heated and melted, and continuously stirred;
s2: maintaining the temperature at 65-75 ℃, slowly adding 280-290 parts of phosphorus pentoxide step by step within 110-130 minutes, and maintaining the temperature to continue reacting for 2 hours;
s3: maintaining the temperature at 65-70 ℃, adding 150-160 parts of oleic acid and 85-90 parts of triethanolamine to react for 30min, adding 80-90 parts of tween 80 and 165-170 parts of sorbitol, and stirring for 10min;
s4: adding 1725-1750 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; sequentially adding 360-370 parts of 50% sodium acetate solution at the temperature, stirring for 10min, adding 340-350 parts of 35% sodium hydroxide solution, stirring for 10min, adding 295-300 parts of sodium acetate, and stirring for 10min;
s5: and adding 14-30 parts of 35% sodium hydroxide, adjusting the pH to 8.0-8.5, and obtaining the phosphate fatliquor, wherein the solid content is 48-52%.
In a preferred embodiment, the preparation process of the alkylolamides is:
a1: adding 500-510 parts of oleic acid into a reactor, dissolving 5-8 parts of sodium methoxide by 190-200 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with oleic acid within 45 min;
a2: maintaining the temperature at 140-146 ℃, maintaining the vacuum negative pressure of-0.070 Mpa to-0.090 Mpa, and reacting for 3-3.5h;
a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 175-180 parts of coconut oil acid within 18 min;
a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure of-0.070 Mpa to-0.090 Mpa, and reacting for 5-5.5h to obtain the alkylolamide.
In a preferred embodiment, the method comprises the following steps:
s1: 880 parts of alkylolamide, 540 parts of C12-14 fatty alcohol and 165 parts of polyisobutylene 950 are added into a reactor, heated to melt, and continuously stirred;
s2: maintaining the temperature at 65-75 ℃, slowly adding 280 parts of phosphorus pentoxide step by step within 120 minutes, and continuously reacting for 2 hours while maintaining the temperature;
s3: maintaining the temperature at 65-70 ℃, adding 150 parts of oleic acid and 85 parts of triethanolamine to react for 30min, adding 80 parts of tween 80 and 165 parts of sorbitol, and stirring for 10min;
s4: adding 1725 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; sequentially adding 370 parts of 50% sodium acetate solution at the temperature, stirring for 10min, adding 340 parts of 35% sodium hydroxide solution, stirring for 10min, adding 295 parts of sodium acetate, and stirring for 10min;
s5: and adding 14 parts of 35% sodium hydroxide, adjusting the pH to 8.0, and adjusting the solid content to 48% to obtain the phosphate fatliquor.
In a preferred embodiment, the method comprises the following steps:
s1: 890 parts of alkylolamide, 550 parts of C12-14 fatty alcohol and 170 parts of polyisobutylene 950 are added into a reactor, and the mixture is heated, melted and continuously stirred;
s2: maintaining the temperature at 65-75 ℃, slowly adding 290 parts of phosphorus pentoxide step by step within 110-130 minutes, and continuously reacting for 2 hours while maintaining the temperature;
s3: maintaining the temperature at 65-70 ℃, adding 160 parts of oleic acid and 90 parts of triethanolamine to react for 30min, adding 90 parts of tween 80 and 170 parts of sorbitol, and stirring for 10min;
s4: adding 1750 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; adding 360 parts of 50% sodium acetate solution at the temperature, stirring for 10min, adding 350 parts of 35% sodium hydroxide solution, stirring for 10min, adding 300 parts of sodium acetate, and stirring for 10min;
s5: and adding 30 parts of 35% sodium hydroxide, adjusting the pH to 8.5, and obtaining the phosphate fatliquor with the solid content of 52%.
In a preferred embodiment, the preparation process of the alkylolamides is:
a1: adding 500 parts of oleic acid into a reactor, dissolving 5 parts of sodium methoxide by 190 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with the oleic acid within 45 min;
a2: maintaining the temperature at 140-146 deg.C, and vacuum negative pressure of-0.070 Mpa, and reacting for 3 hr;
a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 175 parts of coconut oil acid within 18 min;
a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure of-0.070 Mpa, and reacting for 5h to obtain the alkylolamide.
In a preferred embodiment, the preparation process of the alkylolamides is:
a1: adding 510 parts of oleic acid into a reactor, dissolving 8 parts of sodium methoxide by 200 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with the oleic acid within 45 min;
a2: maintaining the temperature at 140-146 deg.C, vacuum negative pressure of-0.090 Mpa, and reacting for 3-3.5h;
a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 180 parts of coconut oil acid within 18 min;
a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure at-0.090 Mpa, and reacting for 5.5h to obtain the alkylolamide.
The technical scheme of the invention has the beneficial effects that:
1. the novel synthetic phosphate fatting agent prepared by the invention can improve the fullness, softness and surface hand feeling and moisture of leather.
2. The phosphate ester type fatting agent simultaneously contains high-efficiency multifunctional active substances such as amino, phosphoryl and the like, can react with carboxyl and amino in leather fibers to form a complex with protein, and has good fatting and filling effects, and meanwhile, P = O bonds in phosphate ester functional groups have strong complexation with chromium in leather, so that the synthetic phosphate ester type fatting agent has a long fatting effect on leather, and the leather is soft, full, elastic and moist in hand feeling.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. The embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Example 1
The technical scheme of the invention provides a preparation method of a phosphate fatliquor, which comprises the following steps:
firstly, preparing the alkylolamide, wherein the preparation process comprises the following steps:
a1: adding 500 parts of oleic acid into a reactor, dissolving 5 parts of sodium methoxide by 190 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with the oleic acid within 45 min; a2: maintaining the temperature at 140-146 deg.C, and vacuum negative pressure of-0.070 Mpa, and reacting for 3 hr; a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 175 parts of coconut oil acid within 18 min; a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure of-0.070 Mpa, and reacting for 5h to obtain the alkylolamide.
The prepared alkylolamides are used in the next preparation reaction and the preparation process is carried out according to the following steps:
s1: 880 parts of alkylolamide, 540 parts of C12-14 fatty alcohol and 165 parts of polyisobutylene 950 are added into a reactor, heated to melt, and continuously stirred;
s2: maintaining the temperature at 65-75 ℃, slowly adding 280 parts of phosphorus pentoxide step by step within 120 minutes, and continuously reacting for 2 hours while maintaining the temperature;
s3: maintaining the temperature at 65-70 ℃, adding 150 parts of oleic acid and 85 parts of triethanolamine to react for 30min, adding 80 parts of tween 80 and 165 parts of sorbitol, and stirring for 10min;
s4: adding 1725 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; at the temperature, 370 parts of 50% sodium acetate solution are sequentially added and stirred for 10min, 340 parts of 35% sodium hydroxide solution is added and stirred for 10min, and 295 parts of sodium acetate is added and stirred for 10min;
s5: and adding 14 parts of 35% sodium hydroxide, adjusting the pH to 8.0, and adjusting the solid content to 48% to obtain the phosphate fatliquor.
Example 2
The technical scheme of the invention provides a preparation method of a phosphate fatliquor, which comprises the following steps:
firstly, preparing the alkylolamide, wherein the preparation process comprises the following steps:
a1: adding 510 parts of oleic acid into a reactor, dissolving 8 parts of sodium methoxide by 200 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with the oleic acid within 45 min; a2: maintaining the temperature at 140-146 deg.C, vacuum negative pressure at-0.090 Mpa, and reacting for 3.5h; a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 180 parts of coconut oil acid within 18 min; a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure at-0.090 Mpa, and reacting for 5.5h to obtain the alkylolamide.
The prepared alkylolamides are used in the next preparation reaction and the preparation process is carried out according to the following steps:
s1: 890 parts of alkylolamide, 550 parts of C12-14 fatty alcohol and 170 parts of polyisobutylene 950 are added into a reactor, and the mixture is heated, melted and continuously stirred;
s2: maintaining the temperature at 65-75 ℃, slowly adding 290 parts of phosphorus pentoxide step by step within 110-130 minutes, and continuously reacting for 2 hours while maintaining the temperature;
s3: maintaining the temperature at 65-70 ℃, adding 160 parts of oleic acid and 90 parts of triethanolamine to react for 30min, adding 90 parts of tween 80 and 170 parts of sorbitol, and stirring for 10min;
s4: adding 1750 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; adding 360 parts of 50% sodium acetate solution at the temperature, stirring for 10min, adding 350 parts of 35% sodium hydroxide solution, stirring for 10min, adding 300 parts of sodium acetate, and stirring for 10min;
s5: and adding 30 parts of 35% sodium hydroxide, adjusting the pH to 8.5, and obtaining the phosphate fatliquor with the solid content of 52%.
Example 3
The technical scheme of the invention provides a preparation method of a phosphate fatliquor, which comprises the following steps:
firstly, preparing the alkylolamide, wherein the preparation process comprises the following steps:
a1: adding 505 parts of oleic acid into a reactor, dissolving 7 parts of sodium methoxide by 190 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with the oleic acid within 45 min; a2: maintaining the temperature at 140-146 deg.C, vacuum negative pressure of-0.080 Mpa, and reacting for 3.2h; a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 177 parts of coconut oil acid within 18 min; a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure of-0.080 Mpa, and reacting for 5.3h to obtain the alkylolamide.
The prepared alkylolamides are used in the next preparation reaction and the preparation process is carried out according to the following steps:
s1: adding 885 parts of alkylolamide, 550 parts of C12-14 fatty alcohol and 160 parts of polyisobutylene 950 into a reactor, heating to melt, and continuously stirring;
s2: maintaining the temperature at 65-75 ℃, slowly adding 280 parts of phosphorus pentoxide step by step within 130 minutes, and continuously reacting for 2 hours while maintaining the temperature;
s3: maintaining the temperature at 65-70 ℃, adding 155 parts of oleic acid and 85 parts of triethanolamine to react for 30min, adding 90 parts of tween 80 and 165 parts of sorbitol, and stirring for 10min;
s4: adding 1750 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; at the temperature, 365 parts of 50 percent sodium acetate solution is added in turn and stirred for 10min, 345 parts of 35 percent sodium hydroxide solution is added and stirred for 10min, 295 parts of sodium acetate is added and stirred for 10min;
s5: and adding 14-30 parts of 35% sodium hydroxide, adjusting the pH to 8.2, and obtaining the phosphate fatliquor with the solid content of 50%.
When the preparation method is used for preparing the alkylolamide, A2 mainly obtains the following two products and a small part of other by-products, and the general formula of the molecular structure of the reaction is as follows:
wherein R1-COOH represents oleic acid.
A3 mainly obtains the following two products and a small part of other byproducts, and the molecular structure general formula of the reaction is as follows:
oleum Cocois and the material
And continuing the reaction to generate a fifth product, wherein the general structural formula of the reaction molecule is as follows:
the final synthetic alkylolamides obtained in A4 are multi-component mixed amides, mainly comprising the above 5 products and some by-products, which, due to their complex composition, contain both single-chain and double-chain products and can impart different properties to the leather when formed into the final product.
The phosphate fat-liquoring agent prepared in the example 1-3 is compared with the fat-liquoring agent 55/C, and the sheep skin is fatliquored, and the specific process is as follows:
naturally drying after the drum comes out, and mechanically softening.
The results of the sensory evaluation of the leather after the fatliquoring are shown in table 1.
| Product(s) | Solid content(％) | Amount (%) | Fullness and fullness of skin | Softness | Surface hand feeling |
| 55/C | 50 | 10 | 5 | 5 | 5 |
| Example 1 | 49.68 | 10 | 5.5 | 6.5-7.0 | 6.5 |
| Example 2 | 49.95 | 10 | 5.5 | 6.5 | 6.5 |
| Example 3 | 48.95 | 10 | 5.5 | 6.5 | 6.5 |
TABLE 1
It can be seen from the data in the table that the fullness of the examples 1, 2 and 3 is slightly better than that of the comparative sample; however, in the case, the novel synthetic phosphate fatliquor simultaneously contains active ingredients such as amino, phosphoryl and the like, which is more favorable for acting with carboxyl and amino in leather fibers and forming a complex with protein, so that the softness and surface hand feeling of cases 1, 2 and 3 are better than those of a comparative sample.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by one of ordinary skill in this and related arts based on the embodiments of the present invention without creative efforts, shall fall within the protection scope of the present invention. Structures, devices, and methods of operation not specifically described or illustrated herein are generally practiced in the art without specific recitation or limitation.
Claims (5)
1. The preparation method of the phosphate fatliquor is characterized by comprising the following steps:
s1: 880-890 parts of alkylolamides, 540-550 parts of C12-14 fatty alcohols and 160-170 parts of polyisobutylene 950 are added into a reactor, heated and melted, and continuously stirred;
s2: maintaining the temperature at 65-75 ℃, slowly adding 280-290 parts of phosphorus pentoxide step by step within 110-130 minutes, and maintaining the temperature to continue reacting for 2 hours;
s3: maintaining the temperature at 65-70 ℃, adding 150-160 parts of oleic acid and 85-90 parts of triethanolamine to react for 30min, adding 80-90 parts of tween 80 and 165-170 parts of sorbitol, and stirring for 10min;
s4: adding 1725-1750 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; sequentially adding 360-370 parts of 50% sodium acetate solution at the temperature, stirring for 10min, adding 340-350 parts of 35% sodium hydroxide solution, stirring for 10min, adding 295-300 parts of sodium acetate, and stirring for 10min;
s5: adding 14-30 parts of 35% sodium hydroxide, adjusting the pH to 8.0-8.5, and obtaining a phosphate fatliquor, wherein the solid content is 48-52%;
the preparation process of the alkylolamide comprises the following steps:
a1: adding 500-510 parts of oleic acid into a reactor, dissolving 5-8 parts of sodium methoxide by 190-200 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with oleic acid within 45 min;
a2: maintaining the temperature at 140-146 ℃, maintaining the vacuum negative pressure of-0.070 Mpa to-0.090 Mpa, and reacting for 3-3.5h;
a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 175-180 parts of coconut oil acid within 18 min;
a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure of-0.070 Mpa to-0.090 Mpa, and reacting for 5-5.5h to obtain the alkylolamide.
2. The method of preparing a phosphate fatliquor according to claim 1, comprising the steps of:
s1: 880 parts of alkylolamide, 540 parts of C12-14 fatty alcohol and 165 parts of polyisobutylene 950 are added into a reactor, heated to melt, and continuously stirred;
s2: maintaining the temperature at 65-75 ℃, slowly adding 280 parts of phosphorus pentoxide step by step within 120 minutes, and continuously reacting for 2 hours while maintaining the temperature;
s3: maintaining the temperature at 65-70 ℃, adding 150 parts of oleic acid and 85 parts of triethanolamine to react for 30min, adding 80 parts of tween 80 and 165 parts of sorbitol, and stirring for 10min;
s4: adding 1725 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; at the temperature, 370 parts of 50% sodium acetate solution are sequentially added and stirred for 10min, 340 parts of 35% sodium hydroxide solution is added and stirred for 10min, and 295 parts of sodium acetate is added and stirred for 10min;
s5: and adding 14 parts of 35% sodium hydroxide, adjusting the pH to 8.0, and adjusting the solid content to 48% to obtain the phosphate fatliquor.
3. The method of preparing a phosphate fatliquor according to claim 1, comprising the steps of:
s1: 890 parts of alkylolamide, 550 parts of C12-14 fatty alcohol and 170 parts of polyisobutylene 950 are added into a reactor, heated and melted, and continuously stirred;
s2: maintaining the temperature at 65-75 ℃, slowly adding 290 parts of phosphorus pentoxide step by step within 110-130 minutes, and continuously reacting for 2 hours while maintaining the temperature;
s3: maintaining the temperature at 65-70 ℃, adding 160 parts of oleic acid and 90 parts of triethanolamine to react for 30min, adding 90 parts of tween 80 and 170 parts of sorbitol, and stirring for 10min;
s4: adding 1750 parts of 70-75 deg.C hot water within 20min, and maintaining the temperature at 65-75 deg.C; adding 360 parts of 50% sodium acetate solution at the temperature, stirring for 10min, adding 350 parts of 35% sodium hydroxide solution, stirring for 10min, adding 300 parts of sodium acetate, and stirring for 10min;
s5: and adding 30 parts of 35% sodium hydroxide, adjusting the pH to 8.5, and obtaining the phosphate fatliquor with the solid content of 52%.
4. The method for preparing a phosphate fatliquor according to claim 2, characterized in that the preparation process of the alkylolamide is as follows:
a1: adding 500 parts of oleic acid into a reactor, dissolving 5 parts of sodium methoxide by 190 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with the oleic acid within 45 min;
a2: maintaining the temperature at 140-146 deg.C, and vacuum negative pressure of-0.070 Mpa, and reacting for 3 hr;
a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 175 parts of coconut oil acid within 18 min;
a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure of-0.070 Mpa, and reacting for 5h to obtain the alkylolamide.
5. The method for preparing a phosphate fatliquor according to claim 2, characterized in that the preparation process of the alkylolamide is as follows:
a1: adding 510 parts of oleic acid into a reactor, dissolving 8 parts of sodium methoxide by 200 parts of hydroxyethyl ethanolamine in another reactor at the temperature of 80-110 ℃, and then dropwise adding the hydroxyethyl ethanolamine dissolved with the sodium methoxide into the reactor filled with the oleic acid within 45 min;
a2: maintaining the temperature at 140-146 deg.C, vacuum negative pressure of-0.090 Mpa, and reacting for 3-3.5h;
a3: cooling to 110-120 ℃, introducing nitrogen, suspending vacuum negative pressure, and dropwise adding 180 parts of coconut oil acid within 18 min;
a4: maintaining the temperature at 138-142 ℃, maintaining the vacuum negative pressure at-0.090 Mpa, and reacting for 5.5h to obtain the alkylolamide.
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| CN101993961A (en) * | 2009-08-31 | 2011-03-30 | 温州大学 | Amphoteric phosphate fat liquoring agent for leather and preparation method thereof |
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