CN106916088A - A kind of composition, fatting agent and preparation method thereof - Google Patents
A kind of composition, fatting agent and preparation method thereof Download PDFInfo
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- CN106916088A CN106916088A CN201710221515.8A CN201710221515A CN106916088A CN 106916088 A CN106916088 A CN 106916088A CN 201710221515 A CN201710221515 A CN 201710221515A CN 106916088 A CN106916088 A CN 106916088A
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- Prior art keywords
- fatting agent
- esterification products
- agent
- esterification
- maleic anhydride
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- 239000000203 mixture Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 113
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- 238000005886 esterification reaction Methods 0.000 claims abstract description 46
- 230000032050 esterification Effects 0.000 claims abstract description 45
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 31
- 150000003512 tertiary amines Chemical group 0.000 claims abstract description 29
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 25
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims description 13
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 125000003368 amide group Chemical group 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 125000002958 pentadecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 238000006277 sulfonation reaction Methods 0.000 claims 1
- 239000010985 leather Substances 0.000 abstract description 34
- 239000000975 dye Substances 0.000 abstract description 13
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000001804 emulsifying effect Effects 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 238000010792 warming Methods 0.000 description 27
- 239000007787 solid Substances 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000004043 dyeing Methods 0.000 description 12
- 239000000155 melt Substances 0.000 description 11
- 238000009413 insulation Methods 0.000 description 9
- 238000010907 mechanical stirring Methods 0.000 description 9
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 9
- 230000003020 moisturizing effect Effects 0.000 description 9
- 238000010992 reflux Methods 0.000 description 9
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 9
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 6
- 235000010265 sodium sulphite Nutrition 0.000 description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 5
- 239000005642 Oleic acid Substances 0.000 description 5
- 125000000129 anionic group Chemical group 0.000 description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 5
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical class OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 150000008065 acid anhydrides Chemical class 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- AKNUHUCEWALCOI-UHFFFAOYSA-N N-ethyldiethanolamine Chemical class OCCN(CC)CCO AKNUHUCEWALCOI-UHFFFAOYSA-N 0.000 description 3
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 2
- 102000008186 Collagen Human genes 0.000 description 2
- 108010035532 Collagen Proteins 0.000 description 2
- 235000021314 Palmitic acid Nutrition 0.000 description 2
- 235000019483 Peanut oil Nutrition 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- GBAOBIBJACZTNA-UHFFFAOYSA-L calcium sulfite Chemical compound [Ca+2].[O-]S([O-])=O GBAOBIBJACZTNA-UHFFFAOYSA-L 0.000 description 2
- 235000010261 calcium sulphite Nutrition 0.000 description 2
- 229920001436 collagen Polymers 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 230000015784 hyperosmotic salinity response Effects 0.000 description 2
- 229940070765 laurate Drugs 0.000 description 2
- 150000002617 leukotrienes Chemical class 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 239000000312 peanut oil Substances 0.000 description 2
- YCOZIPAWZNQLMR-UHFFFAOYSA-N pentadecane Chemical group CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 1
- 229960000549 4-dimethylaminophenol Drugs 0.000 description 1
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 description 1
- 235000021360 Myristic acid Nutrition 0.000 description 1
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 1
- KYYWBEYKBLQSFW-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCC(O)=O KYYWBEYKBLQSFW-UHFFFAOYSA-N 0.000 description 1
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 125000002960 margaryl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 150000002885 octadecanoids Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- ZTUXEFFFLOVXQE-UHFFFAOYSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCC(O)=O ZTUXEFFFLOVXQE-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
- C07C309/01—Sulfonic acids
- C07C309/02—Sulfonic acids having sulfo groups bound to acyclic carbon atoms
- C07C309/03—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
- C07C309/17—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing carboxyl groups bound to the carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/06—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton from hydroxy amines by reactions involving the etherification or esterification of hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
-
- 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)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
The present invention provides a kind of composition, fatting agent and preparation method thereof, is related to leather production technical field.A kind of fatting agent and the composition for preparing fatting agent, said composition mainly include following components：Aliphatic acid, the hydramine containing tertiary amine groups, maleic anhydride, sulfonating agent.A kind of preparation method of fatting agent, carries out aliphatic acid and hydramine containing tertiary amine groups the first esterification and obtains the first esterification products.First esterification products carry out the second esterification and obtain the second esterification products with maleic anhydride.Second esterification products and sulfonating agent are carried out into sulfonating reaction.This fatting agent emulsifying capacity is strong, good penetrability and leather adhesion are strong.Using functional groups such as carboxyl, tertiary amine groups, sulfonic groups fatting agent can also be made stronger with the adhesion of leather, weaken the competition of fatting agent and dyestuff.Assist dyestuff more preferable to the Color of leather.
Description
Technical field
The present invention relates to leather production technical field, and more particularly to a kind of composition, fatting agent and preparation method thereof.
Background technology
Fatting agent is one of maximum Pi Huacai of consumption in leather production, is had to finished leather performance and its important influence.
Between fatting agent can penetrate into the collagenous fibres of skin, lubrication and plasticization are played, strand segment is easy to motion, finished leather is soft
Soft, waterproof, sun-proof, moist and high resilience.
With widely using for leather and fur products, consumer proposes requirement higher, the coloring of leather to leather and fur products
Emphasis as people's growing interest.Often there is dyeing not poor, dyeing firmness difference of deep, level-dyeing property etc. in the dyeing of current leather
Problem.
The content of the invention
It is an object of the invention to provide a kind of fatting agent, this fatting agent has strong not only emulsifying capacity, good penetrability and skin
The features such as leather adhesion is strong, additionally it is possible to assist dyestuff to the dyeing of leather more firmly, evenly, deeper into leather inside.
Another object of the present invention is to provide a kind of composition for preparing above-mentioned fatting agent, it is utilized respectively containing carboxylic
The component of the functional groups such as base, tertiary amine groups, sulfonic group so that fatting agent is stronger with the adhesion of leather, weakens fatting agent and dyestuff
Competition so that the Color of dyestuff is more preferable.
Another object of the present invention is to provide a kind of preparation method of above-mentioned fatting agent, centered on tertiary amine groups, introduce
Sulfonic group and carboxyl, by adjusting pH value, make fatting agent show cation or anion characteristic, and the stuffing and dyeing for improving leather are imitated
Really.
The present invention is solved its technical problem and is realized using following technical scheme.
The present invention proposes a kind of fatting agent, and its molecular structural formula is：
Wherein, R is alkyl；M is any one in Na, ammonium, Ca, amido.
The present invention proposes a kind of composition for preparing above-mentioned fatting agent.Said composition mainly includes following components：Fat
Fat acid, the hydramine containing tertiary amine groups, maleic anhydride, sulfonating agent.
The present invention proposes a kind of preparation method of above-mentioned fatting agent.Aliphatic acid and hydramine containing tertiary amine groups are carried out into the first ester
Change reaction and obtain the first esterification products；The first esterification products is carried out the second esterification with maleic anhydride and obtain the second esterification product
Thing；And the second esterification products and sulfonating agent are carried out into sulfonating reaction.
The beneficial effect of composition provided in an embodiment of the present invention, fatting agent and preparation method thereof is：
Based on the hydramine containing tertiary amine groups, using carboxyl and the hydroxyl reaction of hydramine of aliphatic acid, aliphatic acid is grafted
Onto tertiary amine groups, leather fiber can be lubricated, reach the purpose for making leather soft.Using the esterification of maleic anhydride and hydramine
Reaction, maleic anhydride is grafted in tertiary amine groups, so as to introduce carboxyl.Carboxyl energy and Cr3+There is coordination and combine in ion, while again
Can be combined with leather collagen fiber, be assigned leather long-acting stuffing effect, so that the tertiary amine groups with weak cation are introduced, and then
The competitive relation between dyestuff and fatting agent is relaxed, the aberration produced after stuffing is solved the problems, such as.In the presence of sulfonating agent, in horse
To introduce sulfonic group on acid anhydrides.Sulfonic group can increase the water solubility and emulsibility of product, and the acidproof or salt tolerance to product has
Certain adjustment effect, can make the dispersion system of product has certain acidproof or salt tolerance.Relative point of the fatting agent
Protonatomic mass is smaller, and in acid condition with electropositive tertiary amine, it is easy to leather inside is permeated for anionic dye is provided
More binding sites, play assisting-dyeing effect.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below will be in the embodiment of the present invention
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional product that can be obtained by commercially available purchase
Product.
Composition provided in an embodiment of the present invention, fatting agent and preparation method thereof are specifically described below.
The embodiment of the present invention provides a kind of fatting agent, and its molecular structural formula is：
Wherein, R is alkyl；M is any one in Na, ammonium, Ca, amido.
More preferably, R is saturated aliphatic chain or unsaturated fatty chain.Specifically, R is undecyl, tridecyl, pentadecane
One kind in base, heptadecyl；M is Na or ammonium.
Wherein, R mainly determines that M is mainly by preparing the fatting agent mistake by preparing the aliphatic acid used during the fatting agent
The sulfonating agent used in journey is determined.
The embodiment of the present invention also provides a kind of composition for preparing above-mentioned fatting agent, and said composition mainly includes following
Component：Aliphatic acid, the hydramine containing tertiary amine groups, maleic anhydride, sulfonating agent.
Composition includes the following components counted by weight：20~28.4 parts of aliphatic acid, the hydramine 8.3 containing tertiary amine groups~
16.9 parts, 6.9~13.9 parts of maleic anhydride, 8.1~17.9 parts of sulfonating agent.
Further, composition includes 23~27 parts of aliphatic acid, the hydramine 10~15 containing tertiary amine groups counted by weight
Part, 8~12 parts of maleic anhydride, 10~16 parts of sulfonating agent.
Using the weak cation of tertiary amine groups in the hydramine containing tertiary amine groups, the competition of fatting agent and anionic dye is reduced,
Enable dyeing of the dyestuff on leather more firm.Fatting agent relative molecular mass is smaller obtained in said composition, is conducive to stuffing
Agent is penetrated into inside leather, for anionic dye provides more binding sites, enables dyeing of the dyestuff on leather deeper.Fat
The introducing of fat acid can make fatting agent lubricate leather fiber, reach the purpose for making leather soft.Introduce sulfonating agent sulfonic group with
Increase the water solubility and emulsibility of fatting agent, increase acidproof, the salt resistance ability of fatting agent.In addition, in composition course of reaction, leading to
Cross maleic anhydride and introduce carboxyl, carboxyl can occur coordination and combine, while can be combined with leather collagen fiber again, assign with chromium ion
Leather long-acting stuffing effect.Be coordinated with reference to when just introduce tertiary amine groups with weak cation and leather and dye contacts, enter
And relax the competitive relation between dyestuff and fatting agent, solve stuffing after produce dyeing loosely the problems such as.
Aliphatic acid can be from laurate (dodecylic acid), myristic acid (tetradecanoic acid), palmitic acid (hexadecanoic acid), hard
Resin acid (octadecanoid acid), oleic acid (9- octadecenoic acids), leukotrienes (9,12,15- octatecatrienoic acids), peanut oil (main bag
Include arachic acid, oleic acid) etc. one or more in various aliphatic acid.
Hydramine containing tertiary amine groups can be from N methyldiethanol amine, N- methyl dipropanolamine, N- ethyldiethanolamines etc.
Hydramine containing two hydroxyls and tertiary amine groups.
Sulfonating agent can select sulphite (such as sodium sulfite, ammonium sulfite, calcium sulfite, organic amine etc.), dense sulphur
Acid, chlorosulfonic acid, sulfur trioxide etc..
The embodiment of the present invention also provides a kind of preparation method of above-mentioned fatting agent.Aliphatic acid and hydramine containing tertiary amine groups are entered
The esterification of row first obtains the first esterification products.Make the first esterification products carry out the second esterification with maleic anhydride again to obtain
Second esterification products.The second esterification products and sulfonating agent are carried out into sulfonating reaction again.
More preferably, aliphatic acid and hydramine containing tertiary amine groups are reacted 7~9 hours in 180~200 DEG C, obtains the first esterification
Product.First esterification products react 4~5 hours with maleic anhydride in 95~105 DEG C, obtain the second esterification products.By the second ester
Change product to be reacted 2~3 hours in 70~80 DEG C with sulfonating agent.
If adding corresponding catalyst in course of reaction, can accordingly shorten the reaction time, for example：Aliphatic acid, containing tertiary amine groups
Hydramine, the first catalyst in 180~200 DEG C react 5~6 hours, obtain the first esterification products.First esterification products and Malaysia
Acid anhydrides, the second catalyst react 2~3 hours in 95~105 DEG C, obtain the second esterification products.Wherein, the first catalyst and second
Catalyst can select the conventional catalyst of esterification, for example ortho phosphorous acid, p-methyl benzenesulfonic acid, dicyclohexylcarbodiimide,
DMAP etc..
Specifically, for example, with aliphatic acid, N methyldiethanol amine, maleic anhydride, sodium sulfite as raw material, ortho phosphorous acid
Used as the first catalyst, p-methyl benzenesulfonic acid prepares fatting agent as the second catalyst.Course of reaction is as follows：
The first step, aliphatic acid and the esterification of N methyldiethanol amine, control aliphatic acid only and N methyldiethanol amine
A hydroxyl reacted.Catalyst ortho phosphorous acid is optionally added into, the addition of catalyst can improve the reaction of the reaction
Speed.The reaction equation of the first step is as follows：
The esterification of second step, maleic anhydride and the first esterification products.Catalyst p-methyl benzenesulfonic acid is optionally added into, is urged
The addition of agent can improve the reaction rate of the reaction.Second step reaction equation is as follows：
3rd step, the second esterification products react with sodium sulfite.Three-step reaction formula is as follows：
More preferably, after the first esterification products temperature is reduced to 75~85 DEG C, maleic anhydride is added and in 95~105 DEG C
Reaction 4~5 hours.Because exothermic phenomenon is had after adding maleic anhydride, therefore, add maleic acid at somewhat lower temperature
Acid anhydride, when temperature rises constant, is further continued for being warming up to and requires that temperature carries out esterification, safer.
In addition, when three-step reaction is carried out, to sulfonating agent (such as 2~5 times) is added in reaction system several times.3rd
The sulfonating reaction of step needs the regular hour, also not anti-because temperature is higher if sulfonating agent disposably is added into reaction system
The sulfonating agent answered is possible to occur the situation of decomposition, causes yield to be difficult to control to.
Alternatively, using being added into again in the reaction system of the 3rd step after hot water dissolving's sulfonating agent.Hot water not only can be with
Accelerate solubility and dissolution velocity of the sulfonating agent in water, meanwhile, it also avoid during by sulfonating agent addition reaction system, reaction
System temperature rapid drawdown, influences being normally carried out (for example, reaction speed is slack-off) for sulfonating reaction.
Alternatively, after the completion of three-step reaction, system being cooled to 50~60 DEG C, moisturizing regulation solid content is 40~
60%, it is 6~8 with NaOH solution (solution of other adjustable pH value can certainly be selected) regulation pH value, obtain fatting agent.Its
In, moisturizing can also further help in the dissolving of sulfonating agent, and sulfonating reaction is also required to be carried out in water phase, make sulfonating reaction
It is more complete.
The pH value requirement of the aqueous dispersion of finished product fatting agent is between 6~8.Through experiment, aqueous dispersion ties up to pH value and is
Less than 5.5, fatting agent can show cationic feature, and pH is lower, and cationic characteristic is obvious.Therefore the pH of product system is adjusted
Section, almost without cationic character, mainly shows anionic character between 6~8.And it is applied to leather processing procedure in fatting agent
When middle, the application process initial stage (application processing body lotion pH value is general 5.5~6.5) needs fatting agent to show anionic property, in the later stage
(due to acid adding reason, pH 3.5~4.0) need fatting agent to show cationic.Therefore, the fatting agent that the present invention is provided can be more
The good requirement for meeting leather processing procedure.
Feature of the invention and performance are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The laurate of 20.0g simultaneously stirs, is warming up to 60 DEG C and melts it, adds 0.20g ortho phosphorous acids, is eventually adding the N- of 11.9g
Methyl diethanolamine, is warming up to 180 DEG C of insulation reactions 6 hours.
(2) treat that system temperature is reduced to 75 DEG C, to the maleic anhydride solid that 9.8g is added in system, treat solid melts
0.10g p-methyl benzenesulfonic acid is added afterwards, and control system temperature is 95 DEG C and reacts 3 hours.
(3) above-mentioned product system is cooled to 60 DEG C, point 2 sodium sulfites of addition 12.6g (add preceding hot water molten
Solution), it is warming up to 70 DEG C and temperature protects reaction 3 hours.50 DEG C are cooled to, moisturizing regulation solid content is 60%, and the NaOH with 30% is molten
Liquid regulation pH value is 6, obtains fatting agent.
Embodiment 2
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The myristic acid of 22.8g simultaneously stirs, is warming up to 65 DEG C and melts it, adds 0.24g ortho phosphorous acids, is eventually adding 11.9g's
N methyldiethanol amine, is warming up to 185 DEG C of insulation reactions 5.8 hours.
(2) treat that system temperature is reduced to 78 DEG C, to the maleic anhydride solid that 9.8g is added in system, treat solid melts
0.12g p-methyl benzenesulfonic acid is added afterwards, and control system temperature is 98 DEG C and reacts 2.8 hours.
(3) above-mentioned product system is cooled to 63 DEG C, point 3 sodium sulfites of addition 12.6g (add preceding hot water molten
Solution), it is warming up to 73 DEG C and temperature protects reaction 2.8 hours.53 DEG C are cooled to, moisturizing regulation solid content is 55%, with 30% NaOH
Solution regulation pH value is 6.5, obtains fatting agent.
Embodiment 3
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The palmitic acid of 25.6g simultaneously stirs, is warming up to 75 DEG C and melts it, adds 0.26g ortho phosphorous acids, is eventually adding the N- of 11.9g
Methyl diethanolamine, is warming up to 190 DEG C of insulation reactions 5.5 hours.
(2) maleic anhydride esterification reaction：Treat that system temperature is reduced to 80 DEG C, to the maleic acid that 9.8g is added in system
Acid anhydride solid, after 0.13g p-methyl benzenesulfonic acid is added after solid melts, control system temperature is 100 DEG C and reacts 2.5 hours.
(3) sulfonating reaction：Above-mentioned product system is cooled to 65 DEG C, point 4 sodium sulfites of addition 12.6g are (before addition
With hot water dissolving), it is warming up to 75 DEG C and temperature protects reaction 2.5 hours.55 DEG C are cooled to, moisturizing regulation solid content is 50%, is used
30% NaOH solution regulation pH value is 7, obtains fatting agent.
Embodiment 4
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The stearic acid of 28.4g simultaneously stirs, is warming up to 85 DEG C and melts it, adds 0.30g ortho phosphorous acids, is eventually adding the N- of 11.9g
Methyl diethanolamine, is warming up to 195 DEG C of insulation reactions 5.3 hours.
(2) treat that system temperature is reduced to 85 DEG C, to the maleic anhydride solid that 9.8g is added in system, treat solid melts
0.15g p-methyl benzenesulfonic acid is added afterwards, and control system temperature is 103 DEG C and reacts 2.2 hours.
(3) above-mentioned product system is cooled to 70 DEG C, the disposable ammonium sulfite for adding 12.6g (adds preceding hot water molten
Solution), it is warming up to 80 DEG C and temperature protects reaction 2 hours.60 DEG C are cooled to, moisturizing regulation solid content is 45%, and the NaOH with 30% is molten
Liquid regulation pH value is 7.5, obtains fatting agent.
Embodiment 5
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The oleic acid of 28.2g is simultaneously stirred, is warming up to 80 DEG C, adds 0.28g ortho phosphorous acids, is eventually adding the N- methyl diethanols of 11.9g
Amine, is warming up to 200 DEG C of insulation reactions 5 hours.
(2) treat that system temperature is reduced to 83 DEG C, to the maleic anhydride solid that 9.8g is added in system, treat solid melts
0.14g p-methyl benzenesulfonic acid is added afterwards, and control system temperature is 105 DEG C and reacts 2 hours.
(3) above-mentioned product system is cooled to 68 DEG C, point 5 ammonium sulfites of addition 12.6g (add preceding hot water molten
Solution), it is warming up to 78 DEG C and temperature protects reaction 2.2 hours.58 DEG C are cooled to, moisturizing regulation solid content is 40%, with 30% NaOH
Solution regulation pH value is 8, obtains fatting agent.
Embodiment 6
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The oleic acid of 20.0g is simultaneously stirred, and is warming up to 85 DEG C.The N methyldiethanol amine of 8.3g is eventually adding, 200 DEG C of insulation reactions are warming up to
9 hours.
(2) to the maleic anhydride solid that 6.9g is added in above-mentioned system, control system temperature is that 105 DEG C of reactions 5 are small
When.
(3) above-mentioned product system is cooled to 60 DEG C, point 6 calcium sulfites of addition 8.1g (add preceding hot water molten
Solution), it is warming up to 78 DEG C and temperature protects reaction 2.5 hours.50 DEG C are cooled to, moisturizing regulation solid content is 30%, and the KOH with 25% is molten
Liquid regulation pH value is 8, obtains fatting agent.
Embodiment 7
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The oleic acid of 10.2g, the palmitic acid of 18.2g are simultaneously stirred, and are warming up to 78 DEG C.The N- methyl dipropanolamines of 16.9g are eventually adding, are heated up
To 180 DEG C of insulation reactions 7 hours.
(2) to the maleic anhydride solid that 13.9g is added in above-mentioned system, control system temperature is that 95 DEG C of reactions 4 are small
When.
(3) above-mentioned product system is cooled to 67 DEG C, point 5 ammonium sulfites of addition 17.9g (add preceding hot water molten
Solution), it is warming up to 78 DEG C and temperature protects reaction 2.5 hours.58 DEG C are cooled to, moisturizing regulation solid content is 30%, uses sodium carbonate liquor
Regulation pH value is 8, obtains fatting agent.
Embodiment 8
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The leukotrienes of 23g, being warming up to 85 DEG C melts it.The N- ethyldiethanolamines of 10g are eventually adding, 180 DEG C of insulations is warming up to anti-
Answer 8 hours.
(2) to the maleic anhydride solid that 8g is added in above-mentioned system, control system temperature is that 100 DEG C of reactions 4.5 are small
When.
(3) above-mentioned product system is cooled to 60 DEG C, point 4 ammonium sulfites (hot water dissolving is used before addition) of addition 10g,
It is warming up to 78 DEG C and temperature protects reaction 2.5 hours.
Embodiment 9
The present embodiment provides a kind of fatting agent, and the preparation method of the fatting agent is as follows：
(1) with thermometer, N2In the isothermal reactor of ingress pipe, reflux condensing tube and mechanical stirring device, add
The peanut oil of 27g, being warming up to 85 DEG C melts it.The N- ethyldiethanolamines of 15g are eventually adding, 180 DEG C of insulations is warming up to anti-
Answer 8 hours.
(2) to the maleic anhydride solid that 12g is added in above-mentioned system, control system temperature is that 100 DEG C of reactions 4.5 are small
When.
(3) above-mentioned product system is cooled to 60 DEG C, point 4 ammonium sulfites (hot water dissolving is used before addition) of addition 16g,
It is warming up to 78 DEG C and temperature protects reaction 2.5 hours.
Comparative example
Anion synthetic fat liquor (model purchased in market：HE, main component is sulfiting neat's foot oil and other natural oils
Synthetic), it is standby.
Test example
Fatting agent prepared by embodiment 1~9 is made into tests below with anion synthetic fat liquor purchased in market.
Fatting agent process of the test prepared by embodiment 1~9 is specific as follows, and the product code numbering that experiment is obtained is respectively 1~9.
The sheep wet blue leather 100g of shaving is taken, specific experiment technique is as follows：
(1) rewetting washing：Water 150g, 30 DEG C, bleeding agent 0.2g rotates 30min, discharge opeing.
(2) neutralize：Water 150g, 30 DEG C, sodium formate 2.0g rotates 20min, sodium bicarbonate (sodium acid carbonate) 0.5g, rotation
40min, regulation pH is 5.5~6.0, discharge opeing.
(3) wash：150g water, rotates 30min discharge opeings by 30 DEG C.
(4) dyeing and stuffing：Water 150g, 50 DEG C, Compound Black 2g rotates 30min.Anion synthetic fat liquor 4g purchased in market, two
Property fatting agent 8g, rotate 60min.
(5) acid adding is fixed：Formic acid (mass fraction is 85%) 1g (is diluted with 10 times of water, added at twice, be spaced
15min), 40min is turned after adding formic acid, pH is 3.5~3.8.Go out drum stand control water, extension dry it is dry, rotary drum fall it is soft after stretched tight
Plate.
Anion synthetic fat liquor purchased in market repeats above-mentioned process of the test, but both sexes stuffing is added without during dyeing and stuffing
Agent, only adds anion synthetic fat liquor 12g purchased in market, and other operating process and parameter are identical.Testing the product code numbering for obtaining is
10。
Result shows, after adding fatting agent, the pliability and feel of 1~No. 10 dry body leather of product are suitable.1~No. 9
Product surface colourity No. 10 product depths of obvious ratio, and color and luster Bearable dry and wet wipe fastness improves 0.5 grade.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of fatting agent, it is characterised in that its molecular structural formula is：
Wherein, R is alkyl；M is any one in Na, ammonium, Ca, amido.
2. fatting agent according to claim 1, it is characterised in that R is saturated aliphatic chain or unsaturated fatty chain.
3. fatting agent according to claim 1, it is characterised in that R is undecyl, tridecyl, pentadecyl, 17
One kind in alkyl；M is Na or ammonium.
4. a kind of composition for preparing fatting agent as any one of claims 1 to 3, it is characterised in that described
Composition mainly includes following components：Aliphatic acid, the hydramine containing tertiary amine groups, maleic anhydride, sulfonating agent.
5. the composition of fatting agent according to claim 4, it is characterised in that the composition includes counting by weight
Following components：20~28.4 parts of aliphatic acid, 8.3~16.9 parts of the hydramine containing tertiary amine groups, 6.9~13.9 parts of maleic anhydride, sulphur
8.1~17.9 parts of agent.
6. the composition of fatting agent according to claim 4, it is characterised in that the composition includes counting by weight
23~27 parts of the aliphatic acid, 10~15 parts of the hydramine containing tertiary amine groups, 8~12 parts of the maleic anhydride, the sulfonation
10~16 parts of agent.
7. the preparation method of a kind of fatting agent as described in any one of claims 1 to 3, it is characterised in that by aliphatic acid and contain
The hydramine of tertiary amine groups carries out the first esterification and obtains the first esterification products；First esterification products are made to be carried out with maleic anhydride
Second esterification obtains the second esterification products；And second esterification products and sulfonating agent are carried out into sulfonating reaction.
8. the preparation method of fatting agent according to claim 7, it is characterised in that by the aliphatic acid and described containing tertiary amine
The hydramine of base reacts 7~9 hours in 180~200 DEG C, obtains first esterification products；First esterification products with it is described
Maleic anhydride reacts 4~5 hours in 95~105 DEG C, obtains second esterification products；By second esterification products with it is described
Sulfonating agent reacts 2~3 hours in 70~80 DEG C.
9. the preparation method of fatting agent according to claim 8, it is characterised in that treat the first esterification products temperature drop
After as little as 75~85 DEG C, add the maleic anhydride and reacted 4~5 hours in 95~105 DEG C.
10. the preparation method of fatting agent according to claim 8, it is characterised in that by the aliphatic acid, described containing tertiary amine
The hydramine of base, the first catalyst react 5~6 hours in 180~200 DEG C, obtain first esterification products；First esterification
Product reacts 2~3 hours with the maleic anhydride, the second catalyst in 95~105 DEG C, obtains second esterification products.
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| CN115368538A (en) * | 2022-09-16 | 2022-11-22 | 四川亭江新材料股份有限公司 | Polyurethane type leather fatting agent and preparation method thereof |
| CN117660705A (en) * | 2023-10-19 | 2024-03-08 | 四川达威科技股份有限公司 | Amphoteric leather fatting agent and preparation method thereof |
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| CN109666769A (en) * | 2019-01-04 | 2019-04-23 | 南雄西顿化工有限公司 | A kind of assisting-dyeing type ring protects amphoteric fatliquor and preparation method thereof |
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| CN117660705A (en) * | 2023-10-19 | 2024-03-08 | 四川达威科技股份有限公司 | Amphoteric leather fatting agent and preparation method thereof |
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Application publication date: 20170704 |