CN115323084A - Silky cationic fatting agent for leather making and preparation method thereof - Google Patents
Silky cationic fatting agent for leather making and preparation method thereof Download PDFInfo
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- CN115323084A CN115323084A CN202210950533.0A CN202210950533A CN115323084A CN 115323084 A CN115323084 A CN 115323084A CN 202210950533 A CN202210950533 A CN 202210950533A CN 115323084 A CN115323084 A CN 115323084A
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- silky
- cationic
- acid
- tanning
- emulsifier
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- 125000002091 cationic group Chemical group 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000010985 leather Substances 0.000 title abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000839 emulsion Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 238000004945 emulsification Methods 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N p-toluenesulfonic acid Substances CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 2
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 125000005489 p-toluenesulfonic acid group Chemical group 0.000 claims description 2
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 2
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 2
- 229920000136 polysorbate Polymers 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003792 electrolyte Substances 0.000 abstract description 3
- 239000000835 fiber Substances 0.000 abstract description 3
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- 125000003277 amino group Chemical group 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 150000001768 cations Chemical class 0.000 description 6
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- CKLJMWTZIZZHCS-UHFFFAOYSA-N D-OH-Asp Natural products OC(=O)C(N)CC(O)=O CKLJMWTZIZZHCS-UHFFFAOYSA-N 0.000 description 3
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 2
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 2
- 235000013922 glutamic acid Nutrition 0.000 description 2
- 239000004220 glutamic acid Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- REIUXOLGHVXAEO-UHFFFAOYSA-N pentadecan-1-ol Chemical compound CCCCCCCCCCCCCCCO REIUXOLGHVXAEO-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- -1 alcohol amine Chemical class 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 150000002148 esters Chemical group 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
The invention relates to a silky cationic fatting agent for tanning and a preparation method thereof, wherein the preparation method comprises the following steps: and (2) carrying out synthetic reaction on amino dibasic acid and higher alcohol in the presence of a catalyst, adding acid to neutralize until the pH value is 3-5, and then adding an emulsifier, white oil and water to carry out an emulsification reaction to obtain the cationic fatliquor. The fatting agent prepared by the method has amino groups in the structure, provides better cationic performance under an acidic condition, has good adhesion with leather fibers, is not easy to elute, has excellent surface fatting effect, excellent electrolyte resistance and soft and silky feeling of surface fatting, good appearance sale of products, white emulsion, good fluidity, extremely easy emulsification of cold water and hot water, convenient taking and use, and the method is simple and stable, easy to realize, free of pollution, and free of harmful solvent participation and waste discharge.
Description
Technical Field
The invention belongs to the technical field of fatting agents, and particularly relates to a silky cationic fatting agent for leather making and a preparation method thereof.
Background
Leather greasing is one of the important steps in leather production, and is to treat leather with greasing agent to make leather absorb certain amount of grease and endow leather with certain physical and mechanical performance and use 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, dye and fix color and slow down the outward migration of the tanning agent. The main medicine of the leather fatting agent consists of neutral oil and emulsified components, the fat components in the fatting agent are different, and the leather treated by the fatting agent has different styles.
The fatting agents in the prior art are generally divided into two types, one is that oil phase substances such as chlorinated liquid wax and the like are uniformly mixed to prepare oil phase, and a cationic surfactant, a nonionic emulsifying agent, a stabilizing agent and water are uniformly mixed and emulsified. Slowly adding the oil phase liquid into the water phase liquid, and stirring. The chlorinated alkane contained in the leather is a leather-making restricted substance, and the cation is provided by a cation emulsifier, and is not a true cation fatting agent. The other is prepared by amination or ester exchange of alcohol amine monomers of synthetic oil and natural oil, and emulsifying by cation and nonionic emulsifiers through a certain mechanical method. The cation emulsion prepared by the method has poor penetration and emulsification, unobvious performance and poor preparation stability.
The present invention has been made in view of the above circumstances.
Disclosure of Invention
The cation fatting agent has good binding property with leather fibers, is not easy to elute, has excellent surface fatting effect, excellent electrolyte resistance and surface fatting soft silky feeling, and has simple and stable preparation process and easy manufacture.
The invention provides a preparation method of a silky cationic fatliquor for tanning, which comprises the following steps: carrying out synthetic reaction on amino dibasic acid and higher alcohol under the presence of a catalyst, adding the mixture until the pH is 3-5, and then adding an emulsifier, white oil and water for carrying out an emulsification reaction to obtain the cationic fatliquor;
the reaction equation involved is as follows:
m and n are each an integer of 0 to 3, R is C 6 -C 20 The alkyl group of (1).
Further, the molar ratio of the amino dibasic acid to the higher alcohol is 1.8-2.2.
Furthermore, the temperature of the synthesis reaction is 120-150 ℃, and the synthesis reaction is carried out under the negative pressure of less than 0.06 MPa.
Further, the acid is one or more of formic acid, acetic acid and propionic acid, and the catalyst is p-toluenesulfonic acid or sulfamic acid.
Further, the temperature of neutralization is less than 50 ℃.
Furthermore, the temperature of the emulsification reaction is 80-100 ℃, the reaction time is 1-2h, and the synthesis reaction time is 1.5-2.5h.
Further, the emulsifier is one or more of emulsifier 1305, emulsifier 1307, emulsifier 1308, tween 20, tween 40, tween 60 and tween 80.
Further, the white oil is C 20 -C 30 Branched or linear alkanes of (a).
Furthermore, the addition amount of the emulsifier is 1-3% of the solid content of the emulsion, and the addition amount of the white oil is 10-20% of the solid content of the emulsion.
The invention also provides a leather-making silky cationic fatliquor prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
the fatting agent prepared by the method has amino groups in the structure, provides better cationic performance under an acidic condition, has good adhesion with leather fibers, is not easy to elute, has excellent surface fatting effect, excellent electrolyte resistance and soft and silky feeling of surface fatting, good appearance sale of products, white emulsion, good fluidity, extremely easy emulsification of cold water and hot water, convenient taking and use, and the method is simple and stable, easy to realize, free of pollution, and free of harmful solvent participation and waste discharge.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
The reaction equations in the following examples of the present invention are as follows:
example 1
The preparation method of the silky cationic fatting agent for tanning of the embodiment comprises the following specific steps:
adding amino succinic acid and 1-carbon dodecanol into a reaction kettle according to a molar ratio of 1.
Example 2
The preparation method of the silky cationic fatting agent for tanning provided by the embodiment comprises the following specific steps:
adding glutamic acid and 1-octadecanol into a reaction kettle according to a molar ratio of 1.
Example 3
The preparation method of the silky cationic fatting agent for tanning of the embodiment comprises the following specific steps:
adding the amino succinic acid and 1-carbon pentadecanol into a reaction kettle according to a molar ratio of 1.8, adding a catalyst p-toluenesulfonic acid, evacuating and displacing nitrogen twice, slowly heating until substances in the reaction kettle are molten, starting stirring, starting vacuum to perform negative pressure reaction, wherein the negative pressure is less than 0.06MPa, reacting at 120 ℃ for 2.5 hours, cooling to less than 50 ℃, adjusting the pH value to 3-5 with formic acid, closing vacuum, adding white oil with the solid content of 10% of the emulsion, wherein the white oil is eicosane, adding an emulsifier 1308 with the solid content of 1.5% of the emulsion, tween 80 with the solid content of 1.5% of the emulsion and water, heating to 80 ℃, and performing emulsification reaction for 2 hours to obtain the cationic fatting agent.
Example 4
The preparation method of the silky cationic fatting agent for tanning provided by the embodiment comprises the following specific steps:
adding glutamic acid and 1-octadecanol into a reaction kettle according to a molar ratio of 1.2.
Example 5
The preparation method of the silky cationic fatting agent for tanning provided by the embodiment comprises the following specific steps:
adding amino succinic acid and 1-carbon dodecanol into a reaction kettle according to a molar ratio of 1.
Test example 1
The fat-liquoring agents prepared in examples 1 to 5 were subjected to a fat-liquoring test under the same test conditions, and the specific performance evaluation results are shown in table 1.
TABLE 1
Wherein, the oil-moist feeling is less than 3 without oil dry, 5 points of oil feeling are obvious, the higher the score is, the better the oil-moist feeling is, and the full score is 5 points.
Test example 2
Specific indexes of the fatliquoring agents prepared in examples 1 to 5 of the present invention are shown in table 2.
TABLE 2
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A preparation method of a silky cationic fatting agent for tanning is characterized by comprising the following steps: carrying out synthetic reaction on amino dibasic acid and higher alcohol under the presence of a catalyst, adding acid to neutralize until the pH value is 3-5, and then adding an emulsifier, white oil and water to carry out an emulsification reaction to obtain the cationic fatliquor;
wherein, the reaction equation involved is as follows:
m and n are each an integer of 0 to 3, R is C 6 -C 20 The alkyl group of (1).
2. The method for preparing the silky cationic fatliquor for tanning according to claim 1, characterized in that the molar ratio of the amino dibasic acid to the higher alcohol is 1.8-2.2.
3. The method for preparing the silky cationic fatliquor for tanning according to claim 1, wherein the temperature of the synthesis reaction is 120-150 ℃, the synthesis reaction is carried out under the negative pressure of less than 0.06MPa, and the time of the synthesis reaction is 1.5-2.5h.
4. A method for preparing a silky cationic fatliquor for tanning according to any one of claims 1 to 3, wherein the acid is one or more of formic acid, acetic acid and propionic acid, and the catalyst is p-toluenesulfonic acid or sulfamic acid.
5. A process for the preparation of a silky cationic fatliquor for tanning according to any one of claims 1 to 3, characterised in that the temperature of neutralisation is less than 50 ℃.
6. The method for preparing the silky cationic fatliquor for tanning according to claim 1, wherein the temperature of the emulsification reaction is 80-100 ℃ and the reaction time is 1-2h.
7. The method for preparing the silky cationic fatliquor for tanning according to claim 1, wherein the emulsifier is one or more of emulsifier 1305, emulsifier 1307, emulsifier 1308, tween 20, tween 40, tween 60 and tween 80.
8. The method for preparing the silky cationic fatliquor for tanning according to claim 1, wherein the white oil is C 20 -C 30 Branched or linear alkanes of (a).
9. The method for preparing the silky cationic fatliquor for tanning according to claim 1, wherein the addition amount of the emulsifier is 1-3% of the solid content of the emulsion, and the addition amount of the white oil is 10-20% of the solid content of the emulsion.
10. A silky cationic fatliquor for tanning prepared by the process of any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210950533.0A CN115323084B (en) | 2022-08-09 | 2022-08-09 | Silky cationic fatting agent for leather making and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210950533.0A CN115323084B (en) | 2022-08-09 | 2022-08-09 | Silky cationic fatting agent for leather making and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
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| CN115323084A true CN115323084A (en) | 2022-11-11 |
| CN115323084B CN115323084B (en) | 2023-10-27 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5885474A (en) * | 1995-08-04 | 1999-03-23 | Bayer Aktiengesellschaft | Use of polyaspartic acid amides as leather auxiliary products |
| WO2015107148A1 (en) * | 2014-01-16 | 2015-07-23 | Corichem S.R.L. | Polymeric fatliquors |
| CN104831004A (en) * | 2015-05-30 | 2015-08-12 | 山东黎宁科技新材料有限公司 | Novel synthetic cationic vegetable oil fat liquor and preparation method thereof |
| CN109576417A (en) * | 2018-12-06 | 2019-04-05 | 山东黎宁科技新材料有限公司 | A kind of amino composite tan fatting agent and preparation method thereof |
| CN112679712A (en) * | 2020-12-23 | 2021-04-20 | 齐河力厚化工有限公司 | Synthetic fat liquor, preparation method and application thereof |
| CN113462826A (en) * | 2021-05-24 | 2021-10-01 | 兄弟科技股份有限公司 | Cationic leather fatting agent and preparation method thereof |
-
2022
- 2022-08-09 CN CN202210950533.0A patent/CN115323084B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5885474A (en) * | 1995-08-04 | 1999-03-23 | Bayer Aktiengesellschaft | Use of polyaspartic acid amides as leather auxiliary products |
| WO2015107148A1 (en) * | 2014-01-16 | 2015-07-23 | Corichem S.R.L. | Polymeric fatliquors |
| CN104831004A (en) * | 2015-05-30 | 2015-08-12 | 山东黎宁科技新材料有限公司 | Novel synthetic cationic vegetable oil fat liquor and preparation method thereof |
| CN109576417A (en) * | 2018-12-06 | 2019-04-05 | 山东黎宁科技新材料有限公司 | A kind of amino composite tan fatting agent and preparation method thereof |
| CN112679712A (en) * | 2020-12-23 | 2021-04-20 | 齐河力厚化工有限公司 | Synthetic fat liquor, preparation method and application thereof |
| CN113462826A (en) * | 2021-05-24 | 2021-10-01 | 兄弟科技股份有限公司 | Cationic leather fatting agent and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 崔元臣, 赵永丽, 林国然: "阳离子皮革加脂剂的研制及应用进展", 化学研究, no. 03 * |
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| CN115323084B (en) | 2023-10-27 |
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