High-uniformity fatliquor and preparation method thereof
By carrying out oxidation and sulfation reactions and adjusting the pH value during the preparation process of the leather fatliquor, the problems of poor uniformity and stratification of the existing fatliquor are solved, and a fatliquor with stable performance and high uniformity is prepared. agent to improve the properties of leather.
Patent Information
- Application Number
- CN202411508839.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-28
- Publication Date
- 2025-01-24
AI Technical Summary
The existing oxidized sulfite leather fat-adding agent has poor uniformity and is easy to delaminate after standing, which affects product sales and use.
By passing air into the vegetable oil to perform an oxidation reaction, adding the emulsification reaction solution to perform the sulfation reaction, and adjusting the pH of the reaction solution to 6-8, a fatliquor with high uniformity is prepared.
The prepared lipid agent has good uniformity and emulsification stability, which can maintain no layering for 1 year above 5 ° C, which improves the softness, plumpness and abrasion resistance of the leather.
Smart Images
Figure CN119351638A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of fatliquor in leather chemical materials, in particular to a fatliquor with high uniformity and a preparation method thereof. Background Art
[0002] Leather fatliquor plays an important role in the leather production process. It can not only give leather softness and fullness, but also improve the mechanical strength of leather and make it more wear-resistant. Leather fatliquor is mainly composed of neutral oil and emulsified components. The leather treated with fatliquor has different styles due to different oil components in the fatliquor. However, the oxidized sulfited leather fatliquor on the market is mainly yellow or brown paste liquid. Due to poor uniformity, stratification will occur after standing, affecting subsequent product sales and product use. Summary of the invention
[0003] The object of the present invention is to provide a high-uniformity fatliquor and a preparation method thereof. The fatliquor prepared by the present invention has good uniformity and emulsification stability and can be kept at 5°C or above for 1 year without stratification. The fatliquor is used for fatliquor to give leather high softness, high fullness and more wear-resistant properties.
[0004] In order to achieve the above object, the technical solution adopted by the present invention is: A method for preparing a high-uniformity fatliquor comprises: introducing air into vegetable oil, heating and stirring to carry out an oxidation reaction, adding an emulsified reaction liquid, continuing to heat and stir to carry out a sulfiting reaction, and adjusting the pH of the reaction solution to 6-8 after the reaction is completed.
[0005] Preferably, the vegetable oil comprises any one of rapeseed oil, palm oil and soybean oil.
[0006] Preferably, by weight, the vegetable oil is 90-110 parts, and the emulsified reaction liquid is 40-80 parts.
[0007] Preferably, the emulsified reaction liquid is obtained by mixing sodium dodecyl sulfonate or sodium dodecyl sulfate with a saturated sodium bisulfite solution at 50°C.
[0008] Preferably, the mass ratio of sodium dodecyl sulfonate or sodium dodecyl sulfate to saturated sodium bisulfite solution is 1:5.
[0009] Preferably, the oxidation reaction temperature is 90-120° C., and the oxidation reaction time is 6-10 h.
[0010] Preferably, the sulfitation reaction temperature is 60-90° C., and the sulfitation reaction time is 5-10 h.
[0011] Preferably, an alkaline solution is used to adjust the pH of the reaction solution, and the alkaline solution is obtained by mixing sodium dodecyl sulfonate or sodium dodecyl sulfate with an aqueous triethanolamine solution or dilute ammonia water at 30°C.
[0012] Preferably, the mass ratio of sodium dodecyl sulfonate or sodium dodecyl sulfate to triethanolamine aqueous solution or dilute ammonia water is 1:5.
[0013] The invention also discloses a fatliquor obtained by adopting any of the above methods for preparing a fatliquor with high uniformity.
[0014] Compared with the prior art, the present invention has the following beneficial effects: The method of the invention is simple in process, improves the defect of stratification of the oxidized sulfited leather fatliquor after standing, and improves the uniformity of the fatliquor. The fatliquor prepared by the technology has stable performance; good product fluidity; good emulsification performance, good acid resistance, alkali resistance and chromium resistance stability; when compounded with other fatliquor products, the emulsification and stability of the compounded product can be improved. The leather fatliquored with the fatliquor has good softness, fullness and yellowing resistance. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Figure 1 This is a physical comparison diagram of the fatliquor prepared in Example 1 of the present invention and a commercially available fatliquor; Figure 2 This is a physical picture of the fatliquor prepared in Comparative Example 1 of the present invention; Figure 3 This is a physical picture of the fatliquor prepared in Comparative Example 2 of the present invention. DETAILED DESCRIPTION
[0016] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0017] The embodiment of the present invention provides a method for preparing a highly uniform fatliquor, which comprises: introducing air into vegetable oil, heating and stirring to carry out an oxidation reaction, adding an emulsified reaction liquid, continuing to heat and stir to carry out a sulfiting reaction, and adjusting the pH of the reaction solution to 6-8 after the reaction is completed.
[0018] In some preferred embodiments, the emulsified reaction liquid is obtained by mixing sodium dodecyl sulfate or sodium dodecyl sulfate with a saturated sodium bisulfite solution at 50° C. That is, it is obtained by mixing sodium dodecyl sulfate with a saturated sodium bisulfite solution at 50° C., or by mixing sodium dodecyl sulfate with a saturated sodium bisulfite solution at 50° C.
[0019] In some more preferred embodiments, the mass ratio of sodium dodecyl sulfonate or sodium dodecyl sulfate to saturated sodium bisulfite solution is 1:5.
[0020] In some preferred embodiments, the vegetable oil comprises any one of rapeseed oil, palm oil and soybean oil.
[0021] In some preferred embodiments, the vegetable oil is 90-110 parts by weight, and the emulsified reaction liquid is 40-80 parts by weight.
[0022] In some preferred embodiments, the oxidation reaction temperature is 90-120° C., and the oxidation reaction time is 6-10 h.
[0023] In some preferred embodiments, the sulfitation reaction temperature is 60-90° C., and the sulfitation reaction time is 5-10 h.
[0024] In some preferred embodiments, an alkaline solution is used to adjust the pH of the reaction solution, and the alkaline solution is obtained by mixing sodium dodecyl sulfonate or sodium dodecyl sulfate with an aqueous solution of triethanolamine or dilute ammonia at 30°C. The alkaline solution can be obtained by mixing sodium dodecyl sulfonate with an aqueous solution of triethanolamine at 30°C, or by mixing sodium dodecyl sulfate with dilute ammonia at 30°C, or by mixing sodium dodecyl sulfate with an aqueous solution of triethanolamine at 30°C, or by mixing sodium dodecyl sulfate with dilute ammonia at 30°C.
[0025] In some more preferred embodiments, the mass ratio of sodium dodecyl sulfonate or sodium dodecyl sulfate to triethanolamine aqueous solution or dilute ammonia water is 1:5.
[0026] In order to make the technical solution of the present invention clearer, the preparation method and performance of the high-uniformity fatliquor are described in detail through multiple specific embodiments below.
[0027] Example 1 Preparation method of high uniformity fatliquor: The emulsified reaction liquid is prepared by mixing sodium dodecyl sulfate and saturated sodium bisulfite solution at a mass ratio of (1:5) at 50°C to form a uniform colorless transparent liquid. The alkaline solution is prepared by mixing sodium dodecyl sulfate and triethanolamine aqueous solution at a mass ratio of (1:5) at 30°C to form a uniform colorless transparent liquid. Air is introduced into 100 parts by weight of rapeseed oil, and the temperature is raised and stirred for oxidation reaction, the oxidation reaction temperature is 100°C, and the oxidation reaction time is 10h. Then 60 parts by weight of the emulsified reaction liquid is dissolved, and the temperature is raised and stirred for sulfiting reaction, the sulfiting reaction temperature is 80°C, and the sulfiting reaction time is 10h. Then an alkaline solution is added to adjust the pH value to 7 to obtain a fatliquor with high uniformity.
[0028] The actual picture of the fatliquor prepared in this embodiment is as follows Figure 1 As shown in A.
[0029] Example 2 Preparation method of high uniformity fatliquor: The emulsified reaction liquid is prepared by mixing sodium dodecyl sulfate and saturated sodium bisulfite solution at a mass ratio of (1:5) at 50°C to form a uniform colorless transparent liquid. The alkaline solution is prepared by mixing sodium dodecyl sulfate and triethanolamine aqueous solution at a mass ratio of (1:5) at 30°C to form a uniform colorless transparent liquid. Air is introduced into 100 parts by weight of palm oil, and the temperature is raised and stirred for oxidation reaction, the oxidation reaction temperature is 100°C, and the oxidation reaction time is 10 hours. Then 50 parts by weight of the emulsified reaction liquid is dissolved, and the temperature is continued to be raised and stirred for sulfiting reaction, the sulfiting reaction temperature is 80°C, and the sulfiting reaction time is 10 hours. Then an alkaline solution is added to adjust the pH value to 7.5 to obtain a fatting agent with high uniformity.
[0030] Example 3 Preparation method of high uniformity fatliquor: The emulsified reaction liquid is prepared by mixing sodium dodecyl sulfate and saturated sodium bisulfite solution at a mass ratio of (1:5) at 50°C to form a uniform colorless transparent liquid. The alkaline solution is prepared by mixing sodium dodecyl sulfate and dilute ammonia water at a mass ratio of (1:5) at 30°C to form a uniform colorless transparent liquid. Air is introduced into 100 parts by weight of rapeseed oil, and the temperature is raised and stirred for oxidation reaction, the oxidation reaction temperature is 100°C, and the oxidation reaction time is 10h. Then 60 parts by weight of the emulsified reaction liquid is dissolved, and the temperature is continued to be raised and stirred for sulfiting reaction, the sulfiting reaction temperature is 80°C, and the sulfiting reaction time is 10h. Then an alkaline solution is added to adjust the pH value to 6.5 to obtain a fatliquor with high uniformity.
[0031] Comparative Example 1 The emulsified reaction liquid is prepared by mixing sodium dodecyl sulfate and saturated sodium bisulfite solution at a mass ratio of (1:6) at 50°C to form a uniform colorless transparent liquid. The alkaline solution is prepared by mixing sodium dodecyl sulfate and triethanolamine aqueous solution at a mass ratio of (1:5) at 30°C to form a uniform colorless transparent liquid. Air is introduced into 100 parts by weight of rapeseed oil, and the temperature is raised and stirred for oxidation reaction, the oxidation reaction temperature is 100°C, and the oxidation reaction time is 10h. Then 60 parts by weight of the emulsified reaction liquid is dissolved, and the temperature is raised and stirred for sulfiting reaction, the sulfiting reaction temperature is 80°C, and the sulfiting reaction time is 10h. Then an alkaline solution is added to adjust the pH value to 7.
[0032] The actual picture of the fatliquor prepared in this comparative example is as follows Figure 2 As shown, the fatliquor is turbid as a whole, and there is obvious oil-water stratification.
[0033] Comparative Example 2 The emulsified reaction liquid is prepared by mixing sodium dodecyl sulfate and saturated sodium bisulfite solution at a mass ratio of (1:5) at 50°C to form a uniform colorless transparent liquid. The alkaline solution is prepared by mixing sodium dodecyl sulfate and triethanolamine aqueous solution at a mass ratio of (1:4) at 30°C to form a uniform colorless transparent liquid. Air is introduced into 100 parts by weight of rapeseed oil, and the temperature is raised and stirred for oxidation reaction, the oxidation reaction temperature is 100°C, and the oxidation reaction time is 10h. Then 60 parts by weight of the emulsified reaction liquid is dissolved, and the temperature is raised and stirred for sulfiting reaction, the sulfiting reaction temperature is 80°C, and the sulfiting reaction time is 10h. Then an alkaline solution is added to adjust the pH value to 7.
[0034] The actual picture of the fatliquor prepared in this comparative example is as follows Figure 3 As shown, the fatliquor is turbid as a whole, and there is an obvious solid-liquid stratification phenomenon.
[0035] Test example The fatting agent of Example 1 was compared with the commercially available similar fatting agent (the actual object is shown in the figure). Figure 1 After fatliquoring the wet blue cowhide with a fatliquor dosage of 10% of the hide weight, the leather properties were tested and the results are shown in Table 1.
[0036] Among them, 10% emulsion refers to the emulsion formed by fatliquor and water in a mass ratio of 1:9.
[0037] Leather odor detection method, 10 professionals use their sense of smell to score the natural smell of leather, and the final score is the average. The judging criteria are: Level 1: There is odor; Level 2: There is an odor, but no disturbing odor; Level 3: There is a noticeable odor, but no disturbing odor; Level 4: There is a disturbing odor; Level 5: There is a strong disturbing odor; Level 6: There is an unbearable odor.
[0038] The yellowing resistance of leather is tested using TST-E704 yellowing resistance aging tester, which is divided into 5 levels: Grade 1 - Very bad: The leather has lost its color seriously and the appearance of the leather has changed greatly; Grade 2-Poor: The leather loses color significantly; Grade 3 - Medium: The leather has slightly lost color; Grade 4-Good: The leather has basically no discoloration; Grade 5 - Very good: No color difference in leather.
[0039] Table 1 Performance comparison of the fatliquor of Example 1 and similar fatliquors available on the market .
[0040] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that the technical solutions described in the above embodiments may still be modified, or some or all of the technical features thereof may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for preparing a fatliquor with high uniformity, characterized in that: The method comprises: introducing air into the vegetable oil, heating and stirring to carry out oxidation reaction, adding the emulsified reaction liquid, continuing to heat and stir to carry out sulfiting reaction, and adjusting the pH of the reaction solution to 6-8 after the reaction is completed.
2. The method for preparing a high-uniformity fatliquor according to claim 1, characterized in that: The vegetable oil includes any of rapeseed oil, palm oil and soybean oil.
3. The method for preparing a high-uniformity fatliquor according to claim 1, characterized in that: By weight, the vegetable oil is 90-110 parts, and the emulsified reaction liquid is 40-80 parts.
4. The method for preparing a high-uniformity fatliquor according to claim 1, characterized in that: The emulsified reaction liquid is obtained by mixing sodium dodecyl sulfonate or sodium dodecyl sulfate with a saturated sodium bisulfite solution at 50°C.
5. The method for preparing a high-uniformity fatliquor according to claim 4, characterized in that: The mass ratio of sodium dodecyl sulfonate or sodium dodecyl sulfate to saturated sodium bisulfite solution is 1:
5.
6. The method for preparing a highly uniform fatliquor according to claim 1, characterized in that: The oxidation reaction temperature is 90-120° C., and the oxidation reaction time is 6-10 hours.
7. The method for preparing a highly uniform fatliquor according to claim 1, characterized in that: The sulfiting reaction temperature is 60-90° C., and the sulfiting reaction time is 5-10 hours.
8. The method for preparing a high-uniformity fatliquor according to claim 1, characterized in that: The pH of the reaction solution is adjusted using an alkaline solution, wherein the alkaline solution is obtained by mixing sodium dodecyl sulfonate or sodium dodecyl sulfate with a triethanolamine aqueous solution or dilute ammonia water at 30°C.
9. The method for preparing a highly uniform fatliquor according to claim 8, characterized in that: The mass ratio of sodium dodecyl sulfonate or sodium dodecyl sulfate to triethanolamine aqueous solution or dilute ammonia water is 1:
5.
10. A fatliquor obtained by the method for preparing a fatliquor with high uniformity as claimed in any one of claims 1 to 9.