CN105648125A - Preparation method of polyhydroxyl-modified soybean phosphatide fatliquoring agent - Google Patents
Preparation method of polyhydroxyl-modified soybean phosphatide fatliquoring agent Download PDFInfo
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- CN105648125A CN105648125A CN201610175118.7A CN201610175118A CN105648125A CN 105648125 A CN105648125 A CN 105648125A CN 201610175118 A CN201610175118 A CN 201610175118A CN 105648125 A CN105648125 A CN 105648125A
- Authority
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- China
- Prior art keywords
- mass parts
- soybean phospholipid
- mass
- fatting agent
- hydroxy
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- 235000010469 Glycine max Nutrition 0.000 title claims abstract description 17
- 244000068988 Glycine max Species 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 16
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 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 abstract description 8
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 8
- 235000019253 formic acid Nutrition 0.000 claims abstract description 8
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000008347 soybean phospholipid Substances 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 22
- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims description 17
- 238000010792 warming Methods 0.000 claims description 14
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 11
- -1 poly-hydroxy soybean phospholipid Chemical compound 0.000 claims description 10
- 238000012986 modification Methods 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- LSWYGACWGAICNM-UHFFFAOYSA-N 2-(prop-2-enoxymethyl)oxirane Chemical compound C=CCOCC1CO1 LSWYGACWGAICNM-UHFFFAOYSA-N 0.000 claims description 7
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 229940079827 sodium hydrogen sulfite Drugs 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract 1
- 239000010985 leather Substances 0.000 description 13
- 239000000839 emulsion Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009736 wetting Methods 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)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
The invention relates to a preparation method of a polyhydroxyl-modified soybean phosphatide fatliquoring agent. The soybean phosphatide fatliquoring agent is widely used for fatliquoring at present, while the traditional fatliquoring agent is relatively poor in water solubility and is also not good in filling property. The preparation method comprises the steps of placing 100 parts by mass of soybean phosphatide into a three-neck flask, then, adding 2-2.5 parts by mass of allyl glycidyl ether, heating to 40 DEG C, and reacting at the constant temperature for 2h; adding 5.4-7.7 parts by mass of formic acid into the system, dropwise adding 25-40 parts by mass of hydrogen peroxide within 1h by taking 0.5-1 part by mass of concentrated sulfuric acid as a catalyst, and reacting for 8-10h; heating the system to 75 DEG C, adding 40-65 parts by mass of sodium hydrogen sulfite, and reacting for 3h; and regulating the pH value of the system to 7.5-8 by using 40% NaOH, adding 60-DEG C hot water to regulate the solid content of the system to 60%, and stirring for 30min to obtain the improved fatliquoring agent. The soybean phosphatide fatliquoring agent prepared by using the method disclosed by the invention has better hydrophilicity.
Description
Technical field
The present invention relates to the preparation method of a kind of leather fatting agent, it is specifically related to the preparation method of a kind of poly-hydroxy modified soy bean lipoid leather fat.
Technical background
Fatting agent is one of skin material that in tanning production, consumption is maximum, is also one of important chemical materials in leather processing procedure. It can lubricate leather fiber, prevent leather stiff, cracking, leather can be made again to have corresponding toughness and flexibility, and keep its intensity, it is the important factor affecting leather quality performance.
Crust leather is added fat by soy phospholipids fatting agent, becomes leather soft glossy, and increases thick and plentiful function by the filling of uniqueness, especially that solution leather loose side is useful. But the HLB value of soybean phospholipid is lower, emulsifying property is mainly reflected in lipophilicity, and the oil soluble of soybean phospholipid is fine, water-soluble very poor, is almost insoluble to water. And traditional prepare the water-soluble poor of fatting agent with soybean phospholipid, fillibility is not good yet.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of modified soy bean lipoid fatting agent based on poly-hydroxy, there is better water-soluble and fillibility.
For achieving the above object, the technical solution used in the present invention is:
Step one: the modification of contained Amino End Group in soybean phospholipid:
100 mass parts soybean phospholipids are placed in there-necked flask, then add the glycidyl allyl ether of 2��2.5 mass parts, be warming up to 40 DEG C, isothermal reaction 2h.
Step 2: the oxidate and sulfite modification of soybean phospholipid:
System is added in system the formic acid adding 5.4��7.7 mass parts, taking the vitriol oil of 0.5��1 mass parts as catalyzer, drips in 1h and add 25��hydrogen peroxide of 40 mass parts, reaction 8��10h. System is warming up to 75 DEG C, adds 40��65 mass parts sodium bisulfites, reaction 3h.
Step 3: poly-hydroxy soybean phospholipid fatting agent:
NaOH regulation system pH with 40%, to 7.5��8, adds 60 DEG C of hot water regulation system solid contents to 60%, obtains poly-hydroxy soybean phospholipid fatting agent after stirring 30min.
Compared with prior art, the useful effect of the present invention:
The present invention is by carrying out modification to Amino End Group contained in soybean phospholipid, again unsaturated link(age) contained in soybean phospholipid molecule is carried out oxidate and sulfite modification, containing more hydrophilic hydroxyl and hydrophilic sulfonic group in the soybean phospholipid fatting agent molecule of preparation, there is better wetting ability, easier dispersion and emulsion in aqueous, more be conducive to entering crust leather fiber, thus improve the pliability of crust leather, glossy sense and fillibility etc.
Embodiment
Embodiment 1:
Step one: the soybean phospholipid of 100 mass parts is placed in there-necked flask, then add the glycidyl allyl ether of 2 mass parts, it is warming up to 40 DEG C, isothermal reaction 2h.
Step 2: the formic acid adding 5.8 mass parts in system, taking the vitriol oil of 0.6 mass parts as catalyzer, drips the hydrogen peroxide of the mass parts that adds 30 in 1h, reaction 8h. System is warming up to 75 DEG C, adds 55 mass parts sodium bisulfites, after reaction 3h, obtain poly-hydroxy modified soy bean lipoid fatting agent.
Step 3: the NaOH regulation system pH with 40%, to 7.5��8, adds 60 DEG C of hot water regulation system solid contents to 60%, obtains poly-hydroxy soybean phospholipid fatting agent after stirring 30min.
Embodiment 2:
Step one: the soybean phospholipid of 100 mass parts is placed in there-necked flask, then add the glycidyl allyl ether of 2.3 mass parts, it is warming up to 40 DEG C, isothermal reaction 2h.
Step 2: the formic acid adding 6 mass parts in system, taking the vitriol oil of 0.7 mass parts as catalyzer, drips the hydrogen peroxide of the mass parts that adds 28 in 1h, reaction 8h. System is warming up to 75 DEG C, adds 45 mass parts sodium bisulfites, after reaction 3h, obtain poly-hydroxy modified soy bean lipoid fatting agent.
Step 3: the NaOH regulation system pH with 40%, to 7.5��8, adds 60 DEG C of hot water regulation system solid contents to 60%, obtains poly-hydroxy soybean phospholipid fatting agent after stirring 30min.
Embodiment 3:
Step one: the soybean phospholipid of 100 mass parts is placed in there-necked flask, then add the glycidyl allyl ether of 2.4 mass parts, it is warming up to 40 DEG C, isothermal reaction 2h.
Step 2: the formic acid adding 7.2 mass parts in system, taking the vitriol oil of 0.5 mass parts as catalyzer, drips the hydrogen peroxide of the mass parts that adds 36 in 1h, reaction 9h. System is warming up to 75 DEG C, adds 58 mass parts sodium bisulfites, after reaction 3h, obtain poly-hydroxy modified soy bean lipoid fatting agent.
Step 3: the NaOH regulation system pH with 40%, to 7.5��8, adds 60 DEG C of hot water regulation system solid contents to 60%, obtains poly-hydroxy soybean phospholipid fatting agent after stirring 30min.
Embodiment 4:
Step one: the soybean phospholipid of 100 mass parts is placed in there-necked flask, adds the glycidyl allyl ether of 2.2 mass parts, is warming up to 40 DEG C, isothermal reaction 2h.
Step 2: the formic acid adding 5.6 mass parts in system, taking the vitriol oil of 0.8 mass parts as catalyzer, drips the hydrogen peroxide of the mass parts that adds 28 in 1h, reaction 8h. System is warming up to 75 DEG C, adds 46 mass parts sodium bisulfites, after reaction 3h, obtain poly-hydroxy modified soy bean lipoid fatting agent.
Step 3: the NaOH regulation system pH with 40%, to 7.5��8, adds 60 DEG C of hot water regulation system solid contents to 60%, obtains poly-hydroxy soybean phospholipid fatting agent after stirring 30min.
The poly-hydroxy modified soy bean lipoid fatting agent prepared according to the preparation method of the present invention, compared with traditional modified soy bean lipoid fatting agent, multiple modified soybean phospholipid has more hydrophilic radical, more easily in aqueous systems, form emulsion, it is beneficial to the carrying out of emulsion currying work, easily penetrate into leather fiber inside, thus obtain and good add fat effect.
The content of the present invention is not limited to cited by embodiment, and the conversion of any equivalence that technical solution of the present invention is taked by those of ordinary skill in the art by reading specification sheets of the present invention, the claim being the present invention is contained.
Claims (2)
1. the preparation method of a poly-hydroxy modified soy bean lipoid fatting agent, it is characterised in that:
Realize by following step:
Step one: the modification of contained Amino End Group in soybean phospholipid:
100 mass parts soybean phospholipids are placed in there-necked flask, then add the glycidyl allyl ether of 2��2.5 mass parts, be warming up to 40 DEG C, isothermal reaction 2h;
Step 2: the oxidate and sulfite modification of soybean phospholipid:
System is added in system the formic acid adding 5.4��7.7 mass parts, taking the vitriol oil of 0.5��1 mass parts as catalyzer, drips in 1h and add 25��hydrogen peroxide of 40 mass parts, reaction 8��10h,
System is warming up to 75 DEG C, adds 40��65 mass parts sodium bisulfites, reaction 3h;
Step 3: poly-hydroxy soybean phospholipid fatting agent:
NaOH regulation system pH with 40%, to 7.5��8, adds 60 DEG C of hot water regulation system solid contents to 60%, obtains poly-hydroxy soybean phospholipid fatting agent after stirring 30min.
2. the preparation method of a kind of poly-hydroxy modified soy bean lipoid fatting agent according to claim 1, it is characterised in that:
Realize by following step:
Step one: the modification of contained Amino End Group in soybean phospholipid:
100 mass parts soybean phospholipids are placed in there-necked flask, then add the glycidyl allyl ether of 2��2.5 mass parts, be warming up to 40 DEG C, isothermal reaction 2h;
Step 2: the oxidate and sulfite modification of soybean phospholipid:
System is added in system the formic acid adding 5.4��7.7 mass parts, taking the vitriol oil of 0.5��1 mass parts as catalyzer, drips in 1h and add 25��hydrogen peroxide of 40 mass parts, reaction 8��10h,
System is warming up to 75 DEG C, adds 40��65 mass parts sodium bisulfites, reaction 3h;
Step 3: poly-hydroxy soybean phospholipid fatting agent:
NaOH regulation system pH with 40%, to 7.5��8, adds 60 DEG C of hot water regulation system solid contents to 60%, obtains poly-hydroxy soybean phospholipid fatting agent after stirring 30min.
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CN201610175118.7A CN105648125B (en) | 2016-03-25 | 2016-03-25 | A kind of preparation method of polyhydroxy modified soy bean lipoid fatting agent |
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CN201610175118.7A CN105648125B (en) | 2016-03-25 | 2016-03-25 | A kind of preparation method of polyhydroxy modified soy bean lipoid fatting agent |
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CN105648125A true CN105648125A (en) | 2016-06-08 |
CN105648125B CN105648125B (en) | 2017-09-05 |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106282443A (en) * | 2016-08-18 | 2017-01-04 | 中国皮革和制鞋工业研究院(晋江)有限公司 | A kind of preparation method of phosphate fat-liquoring agent |
CN106755636A (en) * | 2016-11-11 | 2017-05-31 | 陕西科技大学 | Mould proof nano combined fatting agent and preparation method thereof is cooperateed with Nano Silver based on APG |
CN110331236A (en) * | 2019-06-21 | 2019-10-15 | 李新根 | A kind of preparation method of montmorillonite phospholipid composite fat liquor |
CN110616562A (en) * | 2019-09-24 | 2019-12-27 | 陕西科技大学 | Yellowing-resistant perovskite oxide modified soybean oil-based nano composite collagen fiber lubricating material and preparation method thereof |
CN111979365A (en) * | 2020-08-19 | 2020-11-24 | 扬州工业职业技术学院 | Soybean lecithin retanning fatting agent with mildew-proof performance and preparation method thereof |
Citations (2)
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---|---|---|---|---|
US4281997A (en) * | 1979-02-23 | 1981-08-04 | Hoechst Aktiengesellschaft | Process for the greasing of leather and fur skins |
CN102617864A (en) * | 2012-03-31 | 2012-08-01 | 陕西科技大学 | Phosphate leather fat liquoring agent and preparation method thereof |
-
2016
- 2016-03-25 CN CN201610175118.7A patent/CN105648125B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4281997A (en) * | 1979-02-23 | 1981-08-04 | Hoechst Aktiengesellschaft | Process for the greasing of leather and fur skins |
CN102617864A (en) * | 2012-03-31 | 2012-08-01 | 陕西科技大学 | Phosphate leather fat liquoring agent and preparation method thereof |
Non-Patent Citations (1)
Title |
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宋玉卿等: "大豆磷脂改性技术综述", 《大豆通报》 * |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106282443A (en) * | 2016-08-18 | 2017-01-04 | 中国皮革和制鞋工业研究院(晋江)有限公司 | A kind of preparation method of phosphate fat-liquoring agent |
CN106282443B (en) * | 2016-08-18 | 2018-07-13 | 中国皮革和制鞋工业研究院(晋江)有限公司 | A kind of preparation method of phosphate fat-liquoring agent |
CN106755636A (en) * | 2016-11-11 | 2017-05-31 | 陕西科技大学 | Mould proof nano combined fatting agent and preparation method thereof is cooperateed with Nano Silver based on APG |
WO2018086247A1 (en) * | 2016-11-11 | 2018-05-17 | 陕西科技大学 | Nano-composite fatliquor based on synergistic anti-mould of alkyl glycoside and nano-silver and preparation method therefor |
CN106755636B (en) * | 2016-11-11 | 2019-02-01 | 陕西科技大学 | Mould proof nano combined fatting agent and preparation method thereof is cooperateed with nano silver based on alkyl glycosides |
CN110331236A (en) * | 2019-06-21 | 2019-10-15 | 李新根 | A kind of preparation method of montmorillonite phospholipid composite fat liquor |
CN110616562A (en) * | 2019-09-24 | 2019-12-27 | 陕西科技大学 | Yellowing-resistant perovskite oxide modified soybean oil-based nano composite collagen fiber lubricating material and preparation method thereof |
CN111979365A (en) * | 2020-08-19 | 2020-11-24 | 扬州工业职业技术学院 | Soybean lecithin retanning fatting agent with mildew-proof performance and preparation method thereof |
CN111979365B (en) * | 2020-08-19 | 2022-06-14 | 扬州工业职业技术学院 | Soybean lecithin retanning fatting agent with mildew-proof performance and preparation method thereof |
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CN105648125B (en) | 2017-09-05 |
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