CN108546790A - A kind of aging ox-hide leather eases back agent and preparation method thereof - Google Patents
A kind of aging ox-hide leather eases back agent and preparation method thereof Download PDFInfo
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- CN108546790A CN108546790A CN201810397126.5A CN201810397126A CN108546790A CN 108546790 A CN108546790 A CN 108546790A CN 201810397126 A CN201810397126 A CN 201810397126A CN 108546790 A CN108546790 A CN 108546790A
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- agent
- leather
- aging
- eases back
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Classifications
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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
Abstract
The present invention relates to a kind of aging ox-hides to remove from office the agent and preparation method thereof that eases back, and belongs to Techniques of Relics Protection field.The present invention is using organosilicon as raw material, silane coupling agent is modifying agent, pass through alkali catalyzed hydrolysis condensation methods synthesizing amino modified organosilicon polysiloxane micro mist, it can be dispersed in amido silicon oil well, and due to the polarity of amino, it can be with the interactions such as hydroxyl, the carboxyl on leather collagen fiber surface, siloxane main chain orientation is set to invest leather collagen fiber surface, it to reduce the friction coefficient between leather, can make to start to slide between leather with the power of very little, fabulous softness, smooth effect can be reached；Fatting agent produced by the present invention all has preferable osmosis to various leather and fur products, it can go deep into inside leather, play repair, leather is set to restore good gas permeability, flexibility, and care agent is less toxic, has no irritating odor, it will not have broad application prospects to leather, human body and environmental concerns after use.
Description
Technical field
The present invention relates to a kind of aging ox-hides to remove from office the agent and preparation method thereof that eases back, and belongs to Techniques of Relics Protection field.
Background technology
Leather cultural relic contains a large amount of history, culture, scientific and technological information, is the wealth of mankind's preciousness.China's archaeology is annual
There are a certain number of leather cultural relics to be exploited, but many since the passage of time faded, stiff, fragile.At present by
In a variety of causes, many leather cultural relics cannot all be effectively protected, and be highly detrimental to its displaying, preserve.In order to make to be unearthed
Leather cultural relic can show elegance in the past, restore a degree of pliability and feel, easing back for reply aging leather is soft
Protection is explored.
Leather and fur products historical relic is the treasure of the Chinese nation, and leather is just utilized by people early in period in time immemorial, makes
It is the material object with important value for reflecting human civilization social development with history much earlier than other textiles.Just because it accumulates
Contain the information such as so abundant history, culture, science and technology, so comparing other historical relics, leather and fur products historical relic more seems more sufficient
It is precious.However, since the main component of leather and fur products is protein, the factors such as the easy light of protein, heat, wet and microorganism influence
And aging and degradation occurs.Therefore, leather quality historical relic is under the influence of various adverse circumstances are long-term, the objects such as moisture content and grease
Matter is gradually lost in, and chief component collagenous fibres also have occurred different degrees of degradation, leather cultural relic becomes to fade, it is thousand hard,
It is mouldy.
Leather cultural relic major part is leather, and leather is formed by rawhide processing tanning, and main component is collagenous fibres, glue
The main chemical compositions of fibrinogen are collagens.Collagen forms 3 α chains by 3 different polypeptide chains again and intermeshes winding
It is in right-handed superhelix structure together.It is longitudinally asymmetric between tropocollagen molecule to be staggered, collagenous fibres are formed, single collagenous fibres are again
Lateral aggregation, and then form the collagenous fiber bundle of bigger.Collagenous fiber bundle point and closes, conjunction and crisscross, spatially netted knot
Structure.This close reticular structure imparts the certain mechanical strength of leather and toughness.Since leather is protein, light,
The effect of the factors such as hot, wet and microorganism, the substances such as moisture and grease in leather can be gradually lost in, and difference can also occur for collagen
The degradation and adhesion of degree lead to leather cultural relic embrittlement, stiffization.At present both at home and abroad to the guarantor that eases back of aging leather and fur products historical relic
Shield is usually used and carries out the method impregnated in water or add fatting agent to leather.Although the research that eases back about leather cultural relic
Retrieval section is in progress, but on the whole, is both at home and abroad still in for the research of this aspect the stage of fumbling, eases back technique not
Enough maturations, the agent type that eases back is single, and the effect that eases back is barely satisfactory, and some can even cause historical relic secondary damage, still there are many
Wait improvements.
Invention content
The technical problems to be solved by the invention：For easing back at present, technique is not mature enough, and the agent type that eases back is single, eases back
The problem of effect is barely satisfactory, and some even can cause secondary damage to historical relic, provide a kind of aging ox-hide leather ease back agent and
Preparation method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of aging ox-hide leather eases back agent, and the agent that eases back includes following weight parts raw material composition：
20~35 parts of fatting agents, 2.5~3.0 parts of emulsifiers, 1~2 part of polysiloxanes micro mist, 5~8 parts of amido silicon oils, 20~30
Part deionized water.
The fatting agent is that lanolin is mixed and heated to 70~80 DEG C with lemon, adds phosphorus pentoxide reaction 2
Warm water hydrolysis is added after~3h, after being cooled to 50~60 DEG C, pH is adjusted to 7~8 for 5% sodium hydroxide solution with mass fraction, then
It is dry to be made to moisture content less than 3%.
The mass ratio of the lanolin and lemon is 16：1~25：1.
The warm water is the deionized water of 70~80 DEG C of temperature, and dosage is 1.0~2.5 times of lanolin quality.
The emulsifier is in neopelex, Tween-80, Span-80, OP-10, polyoxyethylene stearic acid ester
It is one or more.
The polysiloxanes micro mist is aminoethylaminopropyl dimethyl silicone polymer, silane coupling agent HD-109, silane idol
Methyltrimethoxysilane polymeric precipitation is added dropwise in mass fraction is 1% ammonium hydroxide in connection agent HD-110 after mixing, will precipitate water
Ground 200 mesh sieve is made after washing drying.
The aminoethylaminopropyl dimethyl silicone polymer, silane coupling agent HD-109, silane coupling agent HD-110, ammonia
Water, methyltrimethoxysilane parts by weight be 10~15 parts of aminoethylaminopropyl dimethyl silicone polymers, 3.0~4.5 parts of silicon
Alkane coupling agent HD-109,1.0~1.5 parts of silane coupling agent HD-110,600~800 parts of mass fractions are 1% ammonium hydroxide, 200~240
Part methyltrimethoxysilane.
A kind of aging ox-hide removes from office the preparation method for the agent that eases back, the specific steps are：
（1）By aminoethylaminopropyl dimethyl silicone polymer, silane coupling agent HD-109, silane coupling agent HD-110 in quality point
Number is that methyltrimethoxysilane polymeric precipitation is added dropwise after mixing in 1% ammonium hydroxide, by after precipitation washing and drying ground 200
Mesh sieves, and obtains polysiloxanes micro mist；
（2）Lanolin and lemon are mixed and heated to 70~80 DEG C, adds after phosphorus pentoxide reacts 2~3h and temperature is added
Water hydrolyzes, and is that 5% sodium hydroxide solution adjusts pH to 7~8, re-dry to moisture content with mass fraction after being cooled to 50~60 DEG C
Less than 3%, fatting agent is obtained；
（3）Fatting agent, emulsifier, polysiloxanes micro mist, amido silicon oil, deionized water are taken, be fitted into beaker and it is heated to 50~
It 55 DEG C, with 300W 15~20min of microwave treatment, discharges after being cooled to room temperature, obtains aging ox-hide and remove from office the agent that eases back.
Compared with other methods, advantageous effects are the present invention：
（1）For the present invention using organosilicon as raw material, silane coupling agent is modifying agent, is changed by alkali catalyzed hydrolysis condensation methods synthesizing amino
Property organosilicon polysiloxane micro mist, can well be dispersed in amido silicon oil, and due to the polarity of amino, can be fine with leather collagen
The interactions such as hydroxyl, the carboxyl in dimension table face make siloxane main chain orientation invest leather collagen fiber surface, to reduce leather
Between friction coefficient, can make to start to slide between leather with the power of very little, fabulous softness, smooth effect can be reached；
（2）Lotion of the present invention penetrates into collagenous fibres, is filled between collagenous fibres, wherein the polarity of surface active ingredient side
Hydrophilic radical generates chemical bond with tropocollagen molecule side-chain radical, and the oleophylic non-polar group of the other side is consistently back to collagen point
The collagenous fibres of subchain, original close adhesion are opened by " crowded ", and the crosslinking between original collagenous fibres reduces, and is sent out between collagenous fibres
Raw displacement is relatively easy, to, tensile stress and the elongation at break of leather improve, in addition, collagenous fibres are coated by grease, it is main
The compliance of reaction force attenuation between chain and polar side chain, strand is reinforced, and gap becomes larger between collagenous fibres, and collagenous fibres is made to have
Certain free space assigns leather certain flexibility；
（3）Fatting agent produced by the present invention all has preferable osmosis to various leather and fur products, can go deep into inside leather, rises
To repair, leather is made to restore good gas permeability, flexibility, and care agent is less toxic, has no irritating odor, it will not after use
To leather, human body and environmental concerns, have broad application prospects.
Specific implementation mode
Take 10~15g aminoethylaminopropyl dimethyl silicone polymers, 3.0~4.5g silane coupling agents HD-109,1.0~
1.5g silane coupling agent HD-110, be added 600~800g mass fractions be 1% ammonium hydroxide in, with 300~400r/min stirring 1~
2h, then at 0~4 DEG C, 200~240g methyltrimethoxysilane is added dropwise with 1~2g/min, continues stirring 6 after being added dropwise
~8h filters to obtain filter residue, filter residue is washed with deionized 3~5 times, then filter residue is placed in drying box, is done at 70~80 DEG C
It is fitted into grinder and grinds after dry 4~6h, cross 200 mesh sieve, obtain polysiloxanes micro mist, take 80~100g lanolin, 4~5g lemons
Essential oil is fitted into flask, and is heated to 70~80 DEG C, adds 4~12g phosphorus pentoxides, is stirred with 300~400r/min heat preservations
It is 70~80 DEG C of deionized waters the reaction was continued 30~40min to mix and 100~200mL temperature is added after 2~3h, is cooled to 50~60 DEG C
Afterwards, it is that 5% sodium hydroxide solution adjusts pH to 7~8, then is placed in dry to moisture content in drying box and is less than 3% with mass fraction, obtains
Fatting agent, takes 20~35g fatting agents, 2.5~3.0g emulsifiers, 1~2g polysiloxanes micro mists, 5~8g amido silicon oils, 20~
30g deionized waters are fitted into beaker and are heated to 50~55 DEG C, with 300W 15~20min of microwave treatment, go out after being cooled to room temperature
Material obtains aging ox-hide and removes from office the agent that eases back.
Take 10g aminoethylaminopropyl dimethyl silicone polymers, 3.0g silane coupling agents HD-109,1.0g silane coupling agent
HD-110, it is to stir 1h with 300r/min, then at 0 DEG C in 1% ammonium hydroxide that 600g mass fractions, which are added, and 200g is added dropwise with 1g/min
Methyltrimethoxysilane continues to stir 6h after being added dropwise, filters to obtain filter residue, filter residue is washed with deionized 3 times, then will filter
Slag is placed in drying box, is fitted into grinder and is ground after dry 4h at 70 DEG C, crosses 200 mesh sieve, obtain polysiloxanes micro mist, take
80g lanolin, 4g lemons are fitted into flask, and are heated to 70 DEG C, are added 4g phosphorus pentoxides, are kept the temperature with 300r/min
It is 70 DEG C of deionized waters the reaction was continued 30min to stir and 100mL temperature is added after 2h, is 5% with mass fraction after being cooled to 50 DEG C
Sodium hydroxide solution adjusts pH to 7, then is placed in dry to moisture content in drying box and is less than 3%, obtains fatting agent, takes 20g fatting agents,
2.5g emulsifiers, 1g polysiloxanes micro mists, 5g amido silicon oils, 20g deionized waters are fitted into beaker and are heated to 50 DEG C, with
300W microwave treatment 15min, discharge after being cooled to room temperature, and obtain aging ox-hide and remove from office the agent that eases back.
Take 13g aminoethylaminopropyl dimethyl silicone polymers, 3.7g silane coupling agents HD-109,1.3g silane coupling agent
HD-110, it is to stir 1h with 350r/min, then at 2 DEG C, be added dropwise with 1.5g/min in 1% ammonium hydroxide that 700g mass fractions, which are added,
220g methyltrimethoxysilane continues to stir 7h after being added dropwise, filters to obtain filter residue, filter residue is washed with deionized 4 times, then
Filter residue is placed in drying box, is fitted into grinder and grinds after dry 5h at 75 DEG C, cross 200 mesh sieve, obtain polysiloxanes micro mist,
It takes 90g lanolin, 4g lemons to be fitted into flask, and is heated to 75 DEG C, add 8g phosphorus pentoxides, protected with 350r/min
It is 75 DEG C of deionized waters the reaction was continued 35min that 150mL temperature, which is added, after temperature stirring 2h, after being cooled to 55 DEG C, is with mass fraction
5% sodium hydroxide solution adjusts pH to 7, then is placed in dry to moisture content in drying box and is less than 3%, obtains fatting agent, takes 27g stuffings
Agent, 2.7g emulsifiers, 1.5g polysiloxanes micro mists, 6.5g amido silicon oils, 25g deionized waters are fitted into beaker and are heated to 53
DEG C, it with 300W microwave treatment 17min, discharges after being cooled to room temperature, obtains aging ox-hide and remove from office the agent that eases back.
Take 15g aminoethylaminopropyl dimethyl silicone polymers, 4.5g silane coupling agents HD-109,1.5g silane coupling agent
HD-110, it is to stir 2h with 400r/min, then at 4 DEG C in 1% ammonium hydroxide that 800g mass fractions, which are added, and 240g is added dropwise with 2g/min
Methyltrimethoxysilane continues to stir 8h after being added dropwise, filters to obtain filter residue, filter residue is washed with deionized 5 times, then will filter
Slag is placed in drying box, is fitted into grinder and is ground after dry 6h at 80 DEG C, crosses 200 mesh sieve, obtain polysiloxanes micro mist, take
100g lanolin, 5g lemons are fitted into flask, and are heated to 80 DEG C, are added 12g phosphorus pentoxides, are protected with 400r/min
It is 80 DEG C of deionized waters the reaction was continued 40min that 200mL temperature, which is added, after temperature stirring 3h, after being cooled to 60 DEG C, is with mass fraction
5% sodium hydroxide solution adjusts pH to 8, then is placed in dry to moisture content in drying box and is less than 3%, obtains fatting agent, takes 35g stuffings
Agent, 3.0g emulsifiers, 2g polysiloxanes micro mists, 8g amido silicon oils, 30g deionized waters are fitted into beaker and are heated to 55 DEG C, with
300W microwave treatment 20min, discharge after being cooled to room temperature, and obtain aging ox-hide and remove from office the agent that eases back.
The ease back leather agent that eases back of agent and the production of Guangzhou company of aging ox-hide leather prepared by the present invention is detected, is had
Body testing result such as following table table 1：
（1）Pliability is tested：Pliability test is carried out to leather sample using leather softness instrument, not to same sample selection
It is tested and is averaged with putting；
（2）Extension test：Tensile stress and elongation at break test are carried out using fixed weight to leather sample using electronics strength tester
Formula calibrator determination sample thickness.Leather sample is cut out bell-shaped to see, it is 5mm that length, which is 120mm width most thin place, and leather is drawn
It is parallel with ox ridge direction to stretch direction, rate of extension 30cm/min；
（3）Ease back agent emulsion stability test：10mL samples are measured to graduated cylinder, 90mL55~60 DEG C deionized water dissolving is added,
It stirs evenly, is stood under the conditions of 25~35 DEG C for 24 hours, whether there is or not laminations for observation solution；
1 aging ox-hide of table removes from office the agent performance characterization that eases back
The aging ox-hide that as shown in Table 1 prepared by the present invention removes from office the agent that eases back, and aging leather is soft after the processing that eases back for the agent that eases back
Degree is greatly improved, and elongation at break has more apparent raising, and aging ox-hide prepared by the present invention removes from office the agent tool that eases back
There are high market value and application value.
Claims (8)
- The agent 1. a kind of aging ox-hide leather eases back, which is characterized in that the agent that eases back includes following weight parts raw material composition：20~35 parts of fatting agents, 2.5~3.0 parts of emulsifiers, 1~2 part of polysiloxanes micro mist, 5~8 parts of amido silicon oils, 20~30 Part deionized water.
- The agent 2. a kind of aging ox-hide leather as described in claim 1 eases back, which is characterized in that the fatting agent is lanolin and lemon Lemon essential oil is mixed and heated to 70~80 DEG C, adds after phosphorus pentoxide reacts 2~3h and warm water hydrolysis is added, be cooled to 50~60 It is that 5% sodium hydroxide solution adjusts pH to 7~8 with mass fraction, re-dry to moisture content is made less than 3% after DEG C.
- The agent 3. a kind of aging ox-hide leather as claimed in claim 2 eases back, which is characterized in that the lanolin and lemon Mass ratio is 16：1~25：1.
- The agent 4. a kind of aging ox-hide leather as claimed in claim 2 eases back, which is characterized in that the warm water is 70~80 DEG C of temperature Deionized water, dosage is 1.0~2.5 times of lanolin quality.
- The agent 5. a kind of aging ox-hide leather as described in claim 1 eases back, which is characterized in that the emulsifier is detergent alkylate It is one or more in sodium sulfonate, Tween-80, Span-80, OP-10, polyoxyethylene stearic acid ester.
- The agent 6. a kind of aging ox-hide leather as described in claim 1 eases back, which is characterized in that the polysiloxanes micro mist is ammonia second Base aminopropyl dimethyl silicone polymer, silane coupling agent HD-109, silane coupling agent HD-110 are in mass fraction is 1% ammonium hydroxide Methyltrimethoxysilane polymeric precipitation is added dropwise after mixing, ground 200 mesh after precipitation washing and drying is sieved and is made.
- The agent 7. a kind of aging ox-hide leather as claimed in claim 6 eases back, which is characterized in that the poly- diformazan of aminoethylaminopropyl Radical siloxane, silane coupling agent HD-109, silane coupling agent HD-110, ammonium hydroxide, methyltrimethoxysilane parts by weight be 10 ~15 parts of aminoethylaminopropyl dimethyl silicone polymers, 3.0~4.5 parts of silane coupling agent HD-109,1.0~1.5 parts of silane idols Join agent HD-110,600~800 parts of mass fractions are 1% ammonium hydroxide, 200~240 parts of methyltrimethoxysilane.
- The preparation method of agent 8. a kind of aging ox-hide leather as described in claim 1~7 any one eases back, which is characterized in that The specific steps are：（1）By aminoethylaminopropyl dimethyl silicone polymer, silane coupling agent HD-109, silane coupling agent HD-110 in quality point Number is that methyltrimethoxysilane polymeric precipitation is added dropwise after mixing in 1% ammonium hydroxide, by after precipitation washing and drying ground 200 Mesh sieves, and obtains polysiloxanes micro mist；（2）Lanolin and lemon are mixed and heated to 70~80 DEG C, adds after phosphorus pentoxide reacts 2~3h and temperature is added Water hydrolyzes, and is that 5% sodium hydroxide solution adjusts pH to 7~8, re-dry to moisture content with mass fraction after being cooled to 50~60 DEG C Less than 3%, fatting agent is obtained；（3）Fatting agent, emulsifier, polysiloxanes micro mist, amido silicon oil, deionized water are taken, be fitted into beaker and it is heated to 50~ It 55 DEG C, with 300W 15~20min of microwave treatment, discharges after being cooled to room temperature, obtains aging ox-hide and remove from office the agent that eases back.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810397126.5A CN108546790A (en) | 2018-04-28 | 2018-04-28 | A kind of aging ox-hide leather eases back agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810397126.5A CN108546790A (en) | 2018-04-28 | 2018-04-28 | A kind of aging ox-hide leather eases back agent and preparation method thereof |
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| CN108546790A true CN108546790A (en) | 2018-09-18 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735669A (en) * | 2019-02-20 | 2019-05-10 | 朱海鹏 | A kind of leather protection type fatting agent and preparation method thereof |
| CN113604614A (en) * | 2021-09-10 | 2021-11-05 | 西北大学 | Novel hardened leather cultural relic softening agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643801A (en) * | 2008-08-28 | 2010-02-10 | 济南力厚化工有限公司 | Composite synthetic fat liquor and preparation method thereof |
| CN103571982A (en) * | 2013-10-28 | 2014-02-12 | 浙江理工大学 | Method for softening aged leather cultural relic |
| CN104480234A (en) * | 2014-10-27 | 2015-04-01 | 浙江理工大学 | Preparation method of lanolin fatting agent of leather cultural relics |
-
2018
- 2018-04-28 CN CN201810397126.5A patent/CN108546790A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643801A (en) * | 2008-08-28 | 2010-02-10 | 济南力厚化工有限公司 | Composite synthetic fat liquor and preparation method thereof |
| CN103571982A (en) * | 2013-10-28 | 2014-02-12 | 浙江理工大学 | Method for softening aged leather cultural relic |
| CN104480234A (en) * | 2014-10-27 | 2015-04-01 | 浙江理工大学 | Preparation method of lanolin fatting agent of leather cultural relics |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735669A (en) * | 2019-02-20 | 2019-05-10 | 朱海鹏 | A kind of leather protection type fatting agent and preparation method thereof |
| CN113604614A (en) * | 2021-09-10 | 2021-11-05 | 西北大学 | Novel hardened leather cultural relic softening agent and preparation method thereof |
| CN113604614B (en) * | 2021-09-10 | 2022-06-10 | 西北大学 | Plate-bonded leather cultural relic softener and preparation method thereof |
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